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Progress in Natural Science: Materials International 25 (2015) 282290

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Original Research

Texture of the nano-crystalline AlN thin lms and the growth conditions
in DC magnetron sputtering
Shakil Khana,n, Muhammad Shahidb, A. Mahmoodd, A. Shahd, Ishaq Ahmede, Mazhar Mehmooda,
U. Azizd, Q. Razad, M. Alamc
a
Department of Metallurgy and Materials Engineering, Pakistan Institute of Engineering & Applied Sciences, Islamabad, Pakistan
b
Department of Nuclear Engineering, Pakistan Institute of Engineering & Applied Sciences, Islamabad, Pakistan
c
Department of Applied Physics, Pakistan Institute of Engineering & Applied Sciences, Islamabad, Pakistan
d
National Institute of Laser and Optronics (NILOP), Islamabad, Pakistan
e
National Centre for Physics, Quaid-i-Azam University, Islamabad 45320, Pakistan
Received 27 August 2014; accepted 21 December 2014
Available online 11 September 2015

Abstract

DC reactive magnetron sputtering technique has been used for the preparation of AlN thin lms. The deposition temperature and the ow ratio
of N2/Ar were varied and subsequent dependency of the lms crystallites orientation/texture has been addressed. In general, deposited lms were
found hexagonal polycrystalline with a (002) preferred orientation. The X-ray diffraction (XRD) data revealed that the lm crystallinity improves,
with the increase of substrate temperature from 300 1C to 500 1C. The dropped in full width half maximum (FWHM) of the XRD rocking curve
value further conrmed it. However, increasing substrate temperature above 500 1C or reducing the nitrogen condition (from 60 to 30% in the
environment) induced the growth of crystallites with (102) and (103) orientations. The rise of rocking curve FWHM for the corresponding
conditions depicted that the lms texture quality deteriorated. A further conrmation of the variation in lm texture/orentation with the growth
conditions has been obtained from the variation in FWHM values of a dominant E1 (TO) mode in the Fourier transform infrared (FTIR) spectra
and the E2 (high) mode in Raman spectra. We have correlated the columnar structure in AFM surface analyses with the (002) or c-axis orientation
as well. Spectroscopic ellipsometry of the samples have shown a higher refractive index at 500 1C growth temperature.
& 2015 Chinese Materials Research Society. Published by Elsevier GmbH. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).

Keywords: DC reactive magnetron sputtering; XRD; FTIR and Raman spectroscopy

1. Introduction It is known that the physical properties of the lm are

AlN thin lm is a piezoelectric material with a high acoustic
velocity. It is a superior applicant for high frequency devices, like
surface acoustic waves devices (SAW), resonators, high frequency
lters and pressure sensors [13]. The development of wurtzite
(002) or c-axis oriented phase of aluminum nitride (AlN) thin lm
is vital in most of these applications for obtaining higher values of
electromechanical coupling factor k2t [4].
n
Corresponding author.
E-mail address: shakphy@gmail.com (S. Khan).
Peer review under responsibility of Chinese Materials Research Society.
signicantly inuenced by its crystallographic orientation, which
in turn is inuenced by the sputtering process parameters [5]. The
process parameters such as substrate temperature and nitrogen
conditions strongly affect the AlN lm microstructure and
consequently affects SAW propagation velocity and piezoelectric
response [6], i.e. the existence of phases other than the (002)
oriented or c-axis oriented planes results in the deterioration of
SAW propagation velocity and piezoelectric response. Surface
morphology/roughness also plays an important role in applications
such as metallization and wear-resistant coatings [7]. Therefore, to
get AlN lms with desire properties, it is essential to obtain a good
control of the lm crystal quality, preferred orientation and the
transformation from one orientation to other with the variation of

http://dx.doi.org/10.1016/j.pnsc.2015.08.006
1002-0071/& 2015 Chinese Materials Research Society. Published by Elsevier GmbH. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
 S. Khan et al. / Progress in Natural Science: Materials International 25 (2015) 282290 283

growth conditions [8]. So far, many reports on the growth of AlN Shutter control
lms have been published, but no conclusive optimal deposition
parameters have been obtained, and the reports showed difculties
to determine consistent results [9,10]. For example, Verardi et al.
using pulsed laser deposition at 200450 1C on sapphire substrate
[11]. The rise of (002) orientation with the increase in deposition Low Vacuum
pressure from 2
101 to 6
101 Pa and the transformation to gauge Water cooled
cathode
(100) crystal orientation at 8
101 Pa is also reported. Okano
et al. [12] concluded that the growth of c-axis orientated crystal-
lites occurred with the decrease of nitrogen content in the High vacuum line
environment, but Cho [13] and Cheng et al. [14] proposed the
high N2 condition. As far as the substrate temperature is
concerned, Medjani et al. [15] show that lower (below 400 1C) High Vacuum
gauge Substrate holder
temperature is favorable for the formation of (002) plane, however
Jin et al. [16] concluded the 430 1C being the optimum
temperature for the maximum degree of c-axis preferred
orientation. Substrate rotation
The X-ray diffraction (XRD) is a well known technique that
Fig. 1. Experimental setup of magnetron sputtering.
is being frequently used to asses thin lm crystalline orienta-
tion [17]. The other important tools for the microstructure
analysis are the Raman and to some extent Fourier transform Table 1
infra-red spectroscopy (FTIR) [8]. General growth conditions for AlN lms.
In this work, AlN thin lms have been grown by DC reactive Sample description N2/(N2 Ar) (%) Deposition temperature (1C)
magnetron sputtering technique. The inuence of various substrate
temperatures and nitrogen conditions on lm microstructure has Sample A 60 300
been addressed. The lms micro-structural analysis was performed Sample B 60 400
Sample C 60 500
by means of XRD at grazing angle of incidence, XRD rocking Sample D 60 600
curves, FTIR and Raman spectroscopy. The results were corre- Sample E 30 500
lated and obtained an empirical trend for the growth of (002)
oriented AlN lms. The surface feature of the grown lm was Constant parameters (Deposition current and pressure200 mA and 6
10
3
mbar, respectively).
analyzed by atomic force microscopy (AFM) and variation of
morphology was also correlated with the growth conditions.

different substrate temperatures in the range of 300600 1C by

2. Experimental
AlN thin lms were deposited using a balanced DC reactive
magnetron sputtering technique. In the synthesis chamber, a base
vacuum of  104 Pa was achieved using a turbo-molecular pump
(VARIAN Turbo-V-1000 HT) with an average speed of 800 l/sec.
Electronic mass ow controllers (BROOKS mass ow controller
5850 series) was employed for controlled ow of gases. The
substrate temperature during lm growth was measured with the
help of a thermocouple attached to the bottom of a substrate
holder at a distance of 3 cm from target. The Al ux was obtained
from sputtering of Al target (purity: 99.99%). The purity of argon
(Ar) and nitrogen (N2) gases was 99.995%. A schematic diagram
of the apparatus used in this work is shown in Fig. 1.
To evade/reduce contamination of a growing lm, silicon (111)
and quartz substrates were ultrasonically cleaned in acetone/
trichloroethylene for 20 min. In a next step, the substrate was
shadowed from the target by a shutter and its pre-sputtering
wasperformed for 10 min. All the lms were grown without
substrate biasing, keeping the plasma current, cathode voltage and
growth time at 200 mA, 800 V and 40 min, respectively. The
deposition pressure and total gas ow were also kept constant at
6
101 Pa and 10 sccm, respectively. Samples were prepared at
means of resistive heating, while keeping the nitrogen fraction at
60%. Films were also deposited at lower nitrogen condition (30%)
as shown in Table 1. Argon gas was increased in proportion to the
decrease of nitrogen gas and the total pressure during lm growth
was kept constant through an adjustment of a high vacuum valve.
XRD analysis was performed at grazing angle of incidence
using D-8 Discoverer HR-XRD machine equipped with Cu-k
line (1.54 ) source. A parallel beam geometry measurement was
performed at grazing incidence diffraction. To get higher counts
by detector of the XRD machine, the incidence angle () of
primary beam was set as 41 with respect to lm surface. At the
secondary side, a long soller slit was used to limit the radial
divergence to 0.121. To analyze the characteristic spectrum by
functional group, FTIR spectroscopy was performed using Nicolet
6700 FTIR spectrophotometer at an oblique angle (451). Room
temperature Raman spectra of the deposited lms were obtained
via spectroscopic system (Model: MST-4000A; DONG-WOO
OPTRON Co., Ltd.). A IDUS-ANDOR software was use for
collecting the emission spectra in the desired range of wavelength.
The spectroscopic ellipsometric measurements of the lms were
carried out with SENTECH (SE-850) machine equipped with
Xenon lamp. For the investigation of surface features/morphology
of the deposited lms, atomic force microscope (Model: QScope
284 S. Khan et al. / Progress in Natural Science: Materials International 25 (2015) 282290

(002)
(002)

(103)
600 C

Intensity (a.u)
(103)

Intensity (a.u)
(102)
500 C 30%

400 C

300 C 60%

30 40 50 60 70 30 40 50 60 70
2 (degree) 2 (degree)

Fig. 2. XRD spectra of the AlN lms prepared at various (a) substrate temperatures, (b) nitrogen conditions.

350) was employed. All the samples were scanned over an area of Table 2
2
2 mm2 in a taping mode. XRD results for (002) orientation.

Sample Temperature N2/(N2 Ar) FWHM Crystallite size

description (1C) (%) (1) ()
3. Results and discussion
Sample A 300 60 0.590 142
Sample B 400 60 0.30 279
3.1. XRD analysis Sample C 500 60 0.295 284
Sample D 600 60 0.480 174
Investigation of crystalline structure of AlN lms was con- Sample E 500 30 0.246 341
ducted by means of XRD at grazing incidence angle of 41. The
XRD patterns of lms are shown in Fig. 2(a) and (b), as a
function of substrate temperature and percentage nitrogen in the
deposition chamber, respectively. The observed XRD peaks can
be assigned to Wurtzite AlN (Card 01-070-2545) phase. The samples prepared at 300, 400 and 500 1C are 142, 279 and 284
peak at 2 36.0231 can be assign to the (002) orientation, (shown in Table 2), respectively. For the reduced nitrogen
though its position is slightly below the powder data ( 36.041), conditions, the grain size of (002) orientation is slightly higher
which exhibit residual compressive stress in the lm. The ( 341 ) than the grain sizes for the former conditions.
preferred orientation of (002) plane along the surface is clearly To determine the c-axis orientation distribution or textured
evident for the samples prepared at 60% nitrogen, up to a quality of the lms, rocking curve (RC) of (002) diffraction peaks
temperature of 500 1C, above this the relative intensity of (103) were obtained at 2 36.021 in the scan. The RCs of AlN (002)
increases. Furthermore, reducing the nitrogen fraction in the reection at various temperatures are shown in Fig. 3(a). The rise
synthesis chamber induces the growth of (102) and (103) of RC intensity could be seen with the increase of substrate
orientation as well. The XRD spectra also present that the full temperature. The measured full width at half maximum (FWHM)
width at half maximum (FWHM) of (002) reection changes values of the RCs against various temperatures are shown in
with substrate temperature and is shown in Table 2. The FWHM Fig. 3(b). RC of the lm prepared at reduced nitrogen fraction is
of (002) peak was measured using X'pert high score analysis shown in Fig. 3(c) with a 3.9270.151 FWHM value. The lms
software. The measured FWHM values of (002) reection are prepared at 500 1C exhibited the lowest FWHM value depicting
0.5901, 0.301, 0.2951 and 0.4801 at growth temperature of 300, the decrease in orientation distribution and thus the highest textured
400, 500 and 600 1C, respectively. Scherrer's formula of Eq. (1) lm [18]. The higher texture reduced the native defects at grain
could be used to calculate the grain size from XRD pattern [17] boundaries and thus improved the preferred (002) oriented crystal-
line quality.
0:9
t 1 The most stable phase of AlN thin lms is the Wurtzite phase
B cos owing to its close packed structure and (002) orientation has also
where t is the grain size, is the wavelength of measured X-ray been reported to have lowest surface energy [19,20], i.e. surface of
(1.54 ), B is termed as the full width at half maximum (in the lm always has a tendency to lower its energy by growing in
radians) and is the half diffraction angle of crystalline orientation certain texture, which have the lowest possible surface energy and
peak. The calculated average grain sizes of (002) crystallite for the therefore may be a driving force for texture evolution [21]. At
 S. Khan et al. / Progress in Natural Science: Materials International 25 (2015) 282290 285

12

11

10
600 C 9

FWHM (degree)
Intensity (a.u)
8

500 C 7

5
400 C
300 C 4

10 15 20 25 30 300 350 400 450 500 550 600

(degree) Temperature ( C)
Intensity (a.u)

30 %

60 %

10 15 20 25 30
(degree)

Fig. 3. Inuence of temperature on (a) RCs of the AlN lm, (b) FWHM of RCs and (c) inuence of nitrogen fraction on the RC.

300 1C, enough energy was available for islands to nucleate and amorphous. It appeared that when relatively heavier mass ions
grow in (002) orientation and lower their surface energies. Since impinge on substrate surface during lm growth, it imparts more
the adatoms energy strongly depends on the deposition tempera- energy to the depositing species. The adatoms energy thus plays a
ture [22], increasing the growth temperature from 300 1C to key role in determining texture of the deposited AlN lms. As far
500 1C raised the adatoms mobility and surface diffusion length. as the transformation of a highly textured orientation to a mixed
Enhanced mobility enabled adatoms toward lattice sites of the one at lower nitrogen content is concerned, the impact of greater
(002) plane. At 500 1C, generation of vacancies may also numbers of relatively heaver argon ions imparts higher energy to
occurred, which further grew the (002) preferred orientation the depositing species, enabling them to grow in other directions
[23]. The growth could also be related to the interface merging as well, such as [102] and [103].
process induced by substrate temperature. The defects at the grain
or crystallite boundaries exist due to the random orientation of the 3.2. FTIR and Raman analysis
crystallites. At 600 1C, the reduction of (002) crystallites size may
be due to the enhanced desorption rate of the species at substrate FTIR and Raman spectroscopy are important spectroscopic
surface. The re-evaporation from the lm surface decreased the techniques to probe vibrational states of molecules and their
adding probability of species to (002) orientation. Moreover, local order. In this study, the FTIR and Raman analysis were
increasing the substrate temperature further enhanced the adatoms performed to observe the longitudinal optical (LO) and
energy, which enables the (103) orientation to grow as well [23]. transverse optical (TO) phonon vibration modes of AlN thin
Abdallah et al. [24] reported the transformation of lms texture lm and their results were compared to obtain an empirical
from preferred (002) to (100) orientation with the increase of bias relation between them. Group theory predicts eight optical
voltage. The growth of AlN lms at different pressures, at various phonon modes (2A1 2E1 2E2 2B modes) at the point of
N2 Ar gas conditions and at different gas mixtures of nitrogen Brillouine zone of hexagonal AlN. These modes split into the
with other inert gases (neon, krypton and xenon) are also reported longitudinal optical (LO) and transverse optical (TO) compo-
in the literature by different researchers [25,26]. In these reports, nents due to their polar behavior. Among these modes, A1 and
the texture of AlN lms transformed when decreasing the nitrogen E1 are infrared active modes, E2 along with the former modes
fraction in the gas mixture (N2 Ar) and with the increase in are Raman active, while B modes are silent in both. The LO
atomic number of the inert gas, the preferred orientation of AlN modes are active only in the oblique angles analysis [27,28].
lms changes from (002) to (101) orientation, and then to The IR spectral analysis was conducted in a reection mode at
polycrystalline with random orientation and nally became oblique angle (451 off normal). The spectra of the lms were
286 S. Khan et al. / Progress in Natural Science: Materials International 25 (2015) 282290
Absorbance (arb units)
500 600 700
Wavenumber
Fig. 4. Observed FTIR spectra of AlN lm deposited at different (a) temperatures, (b) nitrogen fractions.
obtained in the range of 400 to 1000 cm  1. The effects of
deposition temperature and nitrogen conditions on the FTIR spectra
are presented in Fig. 4(a) and (b), respectively. FTIR spectra of each
gure depict a dominant peak at 673 cm  1 accompanied by a
shoulder peak at 613 cm  1 and a mode at 895 cm  1. Absorption
peaks at 611 cm  1, 672 cm  1 and 895 cm  1 correspond to the A1
(TO), E1 (TO) and A1 (LO) mode of aluminum nitride lm,
respectively [29]. The 620 cm  1 peak arises due to silicon
substrate. The E1 (LO) mode is missing in the FTIR pattern that
is expected to appear at 912 cm  1. The E1 (TO) mode is dominant
in FTIR spectra irrespective of substrate temperature, which
demonstrate that the lms contain mostly (002) or c-axis oriented
crystallites [30]. However, the appearance of a shoulder peak for A1
(TO) mode depicts that crystallites of other phases are also exist and
the (002) crystallites are slightly tilted from surface normal [31].
The decrease in FWHM of FTIR absorption peaks is observable
with the rise in temperature up to 500 1C, as shown in Fig. 4(a). The
decrease in FWHM indicates an improvement in the AlN lm
crystallinity (improvement in the short-range ordering of atoms) [32].
However, further raising the substrate temperature to 600 1C reverses
the trend of peak width, depicting a relatively disordered structure. In
effect, observation of FTIR spectra conrms 500 1C being a relatively
more suitable growth temperature for c-axis oriented AlN lms
grown by DC magnetron sputtering. Observations regarding different
nitrogen growth conditions are shown in Fig. 4(b), depicting a
relatively sharpened peak at 30% nitrogen condition. It appears that at
lower nitrogen content, the crystallites growth of AlN lm occurs. As
the total pressure during deposition was kept constant, reducing the
nitrogen content means a rise of Ar concentration in the plasma
gas. When relatively heavier argon ions impinge on substrate surface,
it transfers more energy to the adatoms, thereby increasing their
mobility. Thus, more coalescent energy is available for relatively
defect-free crystallites in the lm.
Raman spectroscopy is a technologically more important
spectroscopic analysis to probe the vibrational states of crystals
or semiconductors. The measurement was performed using a high
resolution (4 cm  1) Raman spectroscopy system (model MST-
4000A). To avoid overlapping of the AlN peak with silicon
substrate, the Raman analysis was conducted on AlN lms grown
on quartz substrate. Fig. 5 offers the Raman spectra of AlN lms
800 900 500 600 700 800 900
(cm-1) Wavenumber (cm-1)
Intensity (a.u)
500 600 700 800 900 1000
-1
Raman Shift (cm )
Fig. 5. Raman analysis at different growth temperatures.
grown at different substrate temperatures. The spectra of AlN lm
consist of vibrational optical phonon modes at 659 cm  1 and
892 cm  1 corresponding to the transverse optical E2 (high) mode
and A1 (LO) of AlN, respectively [18]. The peak position of E2
mode appears very close to the reported value 657.4 cm  1 [33]
for the un-strained AlN layer. The rise of peak intensity with the
increase of substrate temperature up to 500 1C suggests the local
ordering of crystal structure. The appearance of E2 (high) phonon
mode irrespective of substrate temperature showed that deposited
lms are preferably (002) oriented AlN lm [34] and is in
agreement with XRD and FTIR results. The decrease in FWHM
of observed peak can be seen with the increase in substrate
temperature up to 500 1C that demonstrated lower phonon
scattering effect at grain boundaries and thus lower defects in
lm [26].
3.3. AFM analysis
Atomic force microscopy of the deposited lms was performed
with Model: QScope 350 scanning probe microscope. Fig. 6
shows AFM images of AlN lms depicting the variation of surface
morphology with the increase in substrate temperature. Film prepared
at 300 1C (Fig. 6(a)) depicts only small number of nano-sized
clusters. The number of clusters and packing density increases with
 S. Khan et al. / Progress in Natural Science: Materials International 25 (2015) 282290 287

8.0 8.0
7.0 7.0
6.0 6.0
5.0 5.0
4.0 4.0
8 nm 8 nm
3.0 3.0
2.0 2.0
1.0 1.0

0 0.0 0 0.0
nm nm

500nm 500nm

2000nm 2000nm
1000nm 1000nm
1500nm 1500nm

1000nm 1000nm
1500nm 1500nm
500nm 500nm
2000nm 2000nm
0 0

8.0 8.0
7.0 7.0
6.0 6.0
5.0 5.0
4.0 4.0
8 nm 3.0 8 nm
3.0
2.0 2.0
1.0 1.0
0.0 0.0
0 nm 0 nm

500nm 500nm

2000nm 2000nm
1000nm 1000nm
1500nm 1500nm

1000nm 1000nm
1500nm 1500nm
500nm 500nm

2000nm 2000nm
0 0

Fig. 6. AFM images of AlN lms prepared at (a) 300 1C, (b) 400 1C, (c) 500 1C, and (d) 600 1C.

increase in the substrate temperature up to 400 1C, as shown in Fig. 6
(b). Increasing the substrate temperature to 500 1C has resulted in a
substantially modied surface morphology where a highly textured
surface prole is evident. Computed RMS surface roughness values
were 7, 4, 5 and 6 nm for the lms prepared at 300, 400, 500 and
600 1C respectively. Although RMS roughness does not differ
appreciably, clear indication of substantial surface modication might
result from the change in growth mode. The appearance of columnar
structure in AFM images implies that lms are c-axis oriented as
shown in Fig. 6(c). However, at 600 1C some grooves are produced
within the columnar structure.
At lower substrate temperature (  300 1C), the constituent
particles may not have enough thermal energy to accommodate
themselves at proper position and the growth of crystallites is
therefore multidirectional. Such type of disordered structure
contains higher density of structural defects. At enhanced
substrate temperature of 500 1C, the formation of columnar
structure corresponds to the (002) orientation [32]. The higher
substrate temperature enhances the adatoms mobility and
surface diffusion length. As the most stable phase of AlN
lms is the wurtzite, in a higher adatoms energy conguration,
the most suitable growth for the islands is to grow in c-axis
direction, which is due to its close packed structure and (002)
orientation have the lowest surface energy [19,20]. However,
increasing temperature beyond 500 1C may causes desorption
of the adatoms. The desorption of pits/grooves results in the
formation of clusters as it is clear from Fig. 6(d) within the c-
axis oriented columns.
AFM images of AlN lms prepared at different N2 condi-
tions are shown in Fig. 7(a) and (b). AlN lm deposited at 30%
nitrogen condition (Fig. 7(b)) exhibits a mixed structure of
columns and clusters, suggesting a c-axis orientation along
with other phases as well. The departure of columnar surface
structure to mixed structure of Fig. 7(b) may be attributed to
the difference of argon and nitrogen atomic masses. From the
above analysis, it can be concluded that AFM analysis is
consistent with XRD results.
3.4. Ellipsometry analysis
Ellipsometric measurements of AlN lms were performed to
measure deposited lm thickness and refractive index. The
obtained data was in a form of Psi () and Delta () function,
where represents amplitude ratio while represents the phase
difference between the reected and incident waves. The
measurements were performed at an angle of 701 over a spectral
range from 300 nm to 900 nm. A three layer model was used as
an input in ellipsometry measurement and is shown in Fig. 8(a).
The obtained experimental curves were simulated theoretically
by using multilayered-Cauchy-Urbach model. CauchyUrbach
288 S. Khan et al. / Progress in Natural Science: Materials International 25 (2015) 282290

8.0 8.0
7.0 7.0
6.0 6.0
5.0 5.0
4.0 4.0
8 nm 8 nm
3.0 3.0
2.0 2.0
1.0 1.0
0.0 0.0
0 nm 0 nm

500nm 500nm

2000nm 2000nm
1000nm 1000nm
1500nm 1500nm

1000nm 1000nm
1500nm 1500nm
500nm 500nm
2000nm 2000nm
0 0

Fig. 7. AFM images of AlN lm prepared at N2 condition (a) 60% and (b) 30%.

400
350
300 Psi Exp
Psi Fitted
250
Psi / Delta

Delta Exp
Delta Fitted
200
150
Ambient air 100

AlN(312 nm) 50
SiO 2 0
Si (111) -50
300 400 500 600 700 800 900
Wave Length (nm)

Fig. 8. (a) Multi-Layer model used in ellipsometry, (b) experimental and simulated Psi and Delta curves.

dispersion model utilizes complex refractive index (N n ik) Table 3

whose components i.e. refractive index n() and extinction Ellipsometery results.
coefcients (), are governed by
Sample Temperature N2/ 2 Thickness Refractive index
n n0 C 0 n21 C 1 n42 ::: 2 description (oC) (N2 Ar) (nm) at 2.3 eV
(%)
k1 k2 Sample A 300 60 4.3 322 1.87
k k 0 C0 C1 4 ::: 3
2 Sample B 400 60 3.7 312 1.89
Sample C 500 60 3.8 296 1.90
where n0, n1, and n2 are the refractive indices of ambient, 1st Sample D 600 60 3.2 273 1.88
and 2nd layers respectively, while k0, k1 and k2 represent Sample E 500 30 4.1 369 1.86
extinction coefcient of respective layers. C0 and C1 are
constants with values 102 and 107 respectively. Fig. 8(b)
shows the spectroscopic ellipsometry data together with the
simulated curves for a sample prepared at 400 1C. From where N is the number of data points, Mesi is the ith experimental
Fig. 8(b), it is clear that there is a good agreement between data point, Thi is the ith calculated data point from theoretical
the simulated and experimental data. After sufciently model and i is the standard deviation. The values of mean square
accurate tting was obtained, the lm thickness and refractive errors are shown in Table 3.
indeces were obtained from tted model. The tting was Deposition rates of the deposited lms were calculated from the
analyzed using the mean square error (2) given in Eq. (4) to measured lm thickness and deposition time. The effect of
see the difference of experimental and simulated data. substrate temperature on the deposition rate and refractive indeces
1 XN is shown in Fig. 9(a) and (b), respectively. It appears that
Mesi  Thi 2
2 4 deposition rate of the deposited lms continuously decreases.
N i1 2i The desorption of adatoms from lm surface depend on substrate
 S. Khan et al. / Progress in Natural Science: Materials International 25 (2015) 282290 289

10 1.94

9 1.92

Deposition rate (nm/min)

Refractive index (n)

1.90
8

1.88
7

1.86
6
1.84
5
300 350 400 450 500 550 600 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0 3.2 3.4
Temperature ( C) Photon energy (eV)

Fig. 9. Inuence of substrate temperature on (a) deposition rate, (b) refractive index.

temperature. Increasing the temperature enhances the adatoms [2] A.F. Belyanin, L.L. Bouilov, V.V. Zhirnov, A.I. Kamenev,
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