JOURNAL OF APPLIED PHYSICS

VOLUME 96, NUMBER 6

15 SEPTEMBER 2004

Effect of annealing on refractive indices of radio-frequency magnetron

sputtered waveguiding zinc oxide films on glass
Navina Mehan,a) Vinay Gupta, Kondepudy Sreenivas, and Abhai Mansingh
Department of Physics and Astrophysics, University of Delhi, Delhi-110007, India

(Received 10 March 2004; accepted 27 May 2004)

The effects of annealing and gas composition on the refractive indices of zinc oxide films were
studied in light of the structural properties. ZnO films 1 m were deposited by rf magnetron
sputtering in different oxygen:argon mixtures on glass and annealed at 380 C in air, at different
times. Waveguide modes were excited in the films by prism coupling using a He-Ne laser. The
estimated values of the extraordinary and ordinary refractive indices of the films, which were close
to the corresponding bulk values (ne = 2.006, no = 1.990), initially decreased with annealing time and
later increased before becoming constant with further annealing. The variation in refractive indices
was explained on the basis of contribution from both packing density p and lattice constant c of the
films. The initial decrease in refractive indices was attributed to the observed lattice contraction, and
the latter increase was explained in terms of the increase in packing density (p) of the films on
annealing. A relation is proposed to estimate the refractive indices of films, which have the lattice
constant c different from the bulk value. 2004 American Institute of Physics.
[DOI: 10.1063/1.1774267]
In2O3SnO2 in comparison to bulk and attributed this to
the elongation of the lattice parameter of the films. The observed decrease in the refractive index of the film with annealing was correlated to the lattice contraction without considering the influence of packing density.8
In the present study, ZnO films were deposited by rf
magnetron sputtering on corning glass substrates in different
sputtering gas oxygen:argon O2Ar compositions. The influence of postdeposition annealing at 380 C in air at different
times on the optical and structural properties of the films was
investigated, and the results were analyzed in light of various
factors influencing the refractive index.

I. INTRODUCTION

Zinc oxide ZnO is an interesting material for applications in acousto-optic and electro-optic devices on account of
its electro-optic, elasto-optic, piezoelectric, and optical
waveguiding properties in thin-film form.13 There have been
some reports on the optical properties of ZnO films on glass
deposited by different techniques, in as-grown condition and
after annealing at different temperatures and at different
times.46 However, the results obtained by different workers
vary significantly and are often contradictory, depending on
the fabrication conditions of the films. The refractive indices
of the films are generally observed to be lower than the corresponding bulk values, which is attributed to the lower
packing density in comparison to bulk,4,6 and several models
have been proposed and employed to estimate the packing
density of ZnO films using experimental values of the refractive indices.4,7 However, these models do not consider the
effect of lattice constant on the refractive index. Hickernell,5
as well as Gupta and Mansingh,4 observed an increase in the
refractive indices of rf-sputtered ZnO films up to a certain
annealing temperature (600 C and 400 C, respectively),
which was attributed to the increase in the packing density of
films, whereas the decrease in refractive indices at higher
annealing temperatures was correlated to the presence of microcracks. Contrary to these results, Heideman, Lambeck,
and Gardeniers6 reported a progressive decrease in the refractive index on annealing rf magnetron-sputtered ZnO
films at a fixed temperature 450 C up to 6 h, after which
the refractive index was found to become constant. However,
no attempt was made to explain these results. Dietrich
Schmalzbauer, and Hoffman8 reported a higher value of refractive indices of as-deposited indium tin oxide film

II. THEORY

The extraordinary and ordinary refractive indices and

thickness of a waveguiding film can be determined from the
mode effective indices, which are determined using the following equation:9
nef f m = n p sin m ,

where m is the incident angle at which the mth mode is

excited and n p is the refractive index of the rutile prism [n p
= 2.8650 in the case of transverse electric (TE) modes and
n p = 2.5837 in the case of transverse magnetic (TM) modes].
The equations for the propagation constants of two excited
TM modes in a film may be solved to give the extraordinary
refractive index and film thickness.9 Similarly, the ordinary
refractive index and film thickness can be determined from
two excited TE modes in the film. In the case of a single
excited mode, the refractive index can be obtained from the
mode effective index using the equation for the propagation
constant of the mode if the film thickness is known.

a)

Electronic mail: navinamehan@yahoo.co.in

0021-8979/2004/96(6)/3134/6/$22.00

3134

2004 American Institute of Physics

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J. Appl. Phys., Vol. 96, No. 6, 15 September 2004

Mehan et al.

3135

TABLE I. Sputtering conditions for the rf magnetron-sputtered zinc oxide

thin films
Target
Substrate
Target substrate distance
Sputtering pressure
Rf power
Substrate temperature
Gas composition O2 : Ar

Zinc Zn99.9% pure

Corning glass 7059
11 cm
1.33 102 m bar
500 W
No heating
Film S1 80: 20
Film S2 60: 40

FIG. 2. Photograph of a streak of guided light in the ZnO film deposited by

rf magnetron sputtering with deposition conditions as in Table I and in the
sputtering gas O2 , Ar ratio 80:20 after annealing at 380 C in air for 1 h.

III. EXPERIMENT

Zinc oxide films of thickness about 1 m were deposited by rf magnetron reactive sputtering on Corning Glass
substrates using a zinc (99.9% pure) target. The chamber was
evacuated to a base pressure of 105 mbar, before allowing
the gases (O2 and Ar) to flow into it. The substrates were
cleaned, prior to sputtering, by in situ plasma etching for
5 min. The films were deposited in two different sputtering
gas O2 : Ar compositions, viz., 80:20 and 60:40, without
changing all other parameters as given in Table I. These are
labeled as films S1 and S2, respectively. The films were
annealed at different temperatures ranging from 50 C to
500 C in air for 1 h, and the waveguiding characteristics of
the films were studied by a setup, using a rutile prism and a
HeNe laser 3 mW, with angular resolution of 0.01. The
propagation loss, measured using an optical fiber 600 m
and a detector with a power meter with resolution 0.01 nW,
was found to decrease on annealing and was minimum
3 dB/ cm for the films annealed at 380 C. Therefore, the
detailed investigation of optical properties was carried out
for the as-grown films and after annealing at the fixed temperature (380 C) in air at different times. The structural
properties of these films were studied by x-ray diffraction
(XRD).
IV. RESULTS AND DISCUSSION

The XRD spectra showed that all the ZnO films are
c-axis oriented. Figure 1 shows the XRD spectrum of the
as-grown film deposited in an O2-Ar ratio 60:40 (film S2).
The XRD peak position values 2 for the as-deposited
films S1 and S2 were 34.01 and 34.30, respectively [bulk
value of 2 = 34.43 (Ref. [10])], and the corresponding values of full width at half maximum (FWHM) of the peaks

FIG. 1. X-ray diffraction (XRD) spectrum of the ZnO film deposited by rf

magnetron sputtering with deposition conditions as in Table I and in the
sputtering gas O2 - Ar ratio 60:40 (film S2).

were 0.46 and 0.20 respectively. Thus, the film deposited

in O2Ar ratio 60:40 was found to have a better crystalline
orientation and a larger grain size (indicated by smaller
FWHM) as compared to the film deposited in O2-Ar ratio
80:20. The crystalline orientation was found to improve in
both the films on annealing, as the values of 2 approached
the corresponding bulk value.
The TM and TE modes were excited in the as-grown and
annealed films, and the extraordinary refractive index nef ,
ordinary refractive index nof and thickness d of the films
were determined (Sec. II). Figure 2 shows a photograph of a
typical streak of guided light observed in the zinc oxide film
annealed for 1 h at 380 C. The representative estimated values of nef , nof , and d for the as-grown films and after annealing at 380 C for 1 h are given in Table II. The symbols S1a
and S2a, respectively, denote the films S1 and S2 after annealing for 1 h. In the symbols, nef m1 , m2, nof m1 m2,
dTMm1 , m2 and dTEm1 , m2, m1 and m2, respectively, represent the order of the two modes from which the corresponding value has been determined. The symbol nof 0 , d
stands for the value of nof determined from the TE mode of
order m = 0 and mean film thickness d, which was estimated
from the excited TM modes in that film. However, the value
of nof for the as-deposited film S1 could not be determined as
the TE modes could not be excited in this film, presumably
due to high loss. The mean values were determined in the
case of more than one value of these parameters for a film,
and these are also given in Table II. The accuracy of the
determination of the refractive index and the thickness of a
film from different modes was within 0.03% and 1%, respectively. It may be noted from Table II that the refractive indices of the films are close to and slightly lower than the corresponding bulk values [neb = 2.006 and nob = 1.990 (Ref.
[11])]. Similarly, the values of nef and nof were also estimated for the films annealed at different times. All these
values are shown in Fig. 3. It is noted from the figure that the
variation of extraordinary and ordinary refractive indices of
both the films (S1 and S2) with annealing time show a similar
behavior, i.e., the refractive indices initially decrease on annealing, and thereafter increase when the annealing time is
increased, before becoming nearly constant with further annealing. It is noted that the initial decrease in the extraordinary refractive index on annealing is more pronounced in the
film deposited in O2 - Ar ratio 80:20 (film S1). For this film,
the refractive index decreased up to an annealing time of 1 h
and for the film S2, up to half an hour. The birefringence

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3136

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J. Appl. Phys., Vol. 96, No. 6, 15 September 2004

TABLE II. Estimated values of the extraordinary refractive index nef, ordinary refractive index nof , and
thickness d of the sputtered ZnO films from the various TM and TE modes, excited and detected in the films

Film

nefm1,m2

Mean value
of nef

nofm1,m2
or nof0,d

dTMm1m2
or dTEm1,m2m

Mean value
of dm

S1

nef0,1 = 1.9854
nef1,2 = 1.9844
nef0,1 = 1.9802
nef1,2 = 1.9792
nef0,1 = 1.9767
nef2,3 = 1.9770

1.9849
0.0005
1.9797
0.0005
1.9769
0.00016

...

1.157

nef0,1 = 1.9782
nef0,1 = 1.9783

1.97825
0.00006

dTM0,1 = 1.154
dTM1,2 = 1.161
dTM0,1 = 0.973
dTM1,2 = 0.979
dTM0,1 = 1.153
dTM2,3 = 1.158
dTE0,1 = 1.150
dTM0,1 = 0.983
dTM1,2 = 0.0983

S2
S1a

S2a

nof0,d = 1.9633
nof0,1 = 1.9568

nof0,d = 1.9592

nef -nof of the films did not change significantly with annealing time, and no definite trend could be observed.
If packing density alone is responsible for the changes in
the refractive indices as observed in some earlier reports,7,4
then the initial decrease in refractive index observed in the
present study (Fig. 3) and by other workers6 may indicate an
unexplained decrease in the packing density on annealing.
On the other hand, Dietrich, Schmalzbauer, and Hoffman8
analyzed the decrease in refractive indices of oxide films
In2O3-SnO2 with annealing in terms of the lattice contraction alone. It is noted from Fig. 4, which shows the variation
of the lattice constant c (estimated from the XRD spectra) of
the ZnO films c f with annealing time, that the lattice constant c of the as-grown films were elongated as compared to
the bulk value cb = 5.2066 ,10 and the elongation was
more prominent in the film S1 deposited in 80% O2. This
indicates the presence of stress in the as-deposited ZnO
films,4,12 which may be caused by defects in film stoichiometry, a mismatch in thermal expansion coefficients of substrate and film, and lattice imperfections like voids and small
grain sizes.13,14 It is noted from the figure that the lattice
constant c f of both the films initially decreased on annealing
to values very close to the bulk value cb = 5.206610, and this
may be attributed to the improvement in stoichiometry of the
films due to reaction of oxygen, diffused from air into the
film, and any oxygen atoms in interstitial sites with Zn in the

FIG. 3. Experimentally estimated values of extraordinary and ordinary refractive indices of ZnO films (nef and nof respectively), deposited by rf
magnetron sputtering with deposition conditions as in Table I and after
annealing at 380 C in air for different times, from excited TM and TE
modes (see Table II).

0.976
1.154

0.983

film to form ZnO, as well as an increase in grain size.15,16 On

annealing for more than 1 h, c f for both the films tended to
saturate toward values below the bulk value (Fig. 4). Thus,
the initial decrease in refractive indices (Fig. 3) may be attributed mainly to the observed contraction of the lattice constant c f (Fig. 4).8 Since the value of c f has attained a saturation value after 1 h, the influence of decrease in porosity
with annealing on refractive indices can safely be assumed to
dominate after the first hour of annealing, leading to the observed increase in refractive indices during this period. These
observations indicate the influence of both lattice constant c f
and packing density on the refractive indices of the films.
Because the lattice constant c f of the as-grown films is
elongated in comparison to that of bulk (Fig. 4), this would
lead to higher refractive indices than that of bulk, as calculated from the expression for refractive indices considering
the effect of a lattice constant alone, given by Dietrich,
Schmalzbauer, and Hoffman8 i.e.,
n f l = nb +

5 n2b 1
c f cb,
2 n bc b

where n f l and nb are, respectively, the refractive indices of

film and bulk, and c f and cb are the corresponding values of
lattice constant c. Because the effect of change in lattice

FIG. 4. Experimentally estimated values of the lattice constant c of ZnO

films c f , deposited by rf magnetron sputtering with deposition conditions
as in Table I and after annealing at 380 C in air at different times, from
XRD spectra.

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Mehan et al.

J. Appl. Phys., Vol. 96, No. 6, 15 September 2004

3137

TABLE III. Theoretical and experimental values of extraordinary refractive index for the as-grown films.
As-deposited film

nef l [using Eq. (2)]

nef (experimental)

Annealing time, th

c f

nef l [using Eq. (3)]

nef (experimental)

S1
S2

2.0765
2.0194

1.9849
1.9797

1.0
0.5

0.0602
0.0147

0.0436
0.0106

0.0080
0.0014

Note: Theoretical values are determined from Dietrichs Eq. (2) using values of c f in Fig. 4. Theoretical values of decrease in extraordinary refractive index
are determined from Eq. (3) and initially observed decrease in lattice constant c f (Fig. 4) in annealing time tnef l and the corresponding experimental
values are nef .

constant c f on birefringence (and hence on anisotropy) was

not substantial, as noted from Fig. 3 and 4, the same expression given by Eq. (2) is assumed to hold for both the extraordinary refractive index (with nb = neb = 2.00611) and the ordinary refractive index (with nb = nob = 1.99011). The values of
extraordinary refractive index for the as-grown films, calculated using Eq. (2) and the values of c f in Fig. 4 nef l are
given in Table III, along with the corresponding experimental
values nef . It is noted that the calculated values nefl are
higher than the bulk value whereas the experimental values
nef are lower than the bulk value, which is attributed to the
lower packing density of the as-deposited films due to the
presence of some porosity. It follows from Eq. (2) that
changes in refractive indices of films on annealing are given
by
n f l = nasg nan =
=

5 n2b 1
casg can
2 n bc b
5 n2b 1
c f ,
2 n bc b

where nasg and nan are respectively the refractive indices of

as grown and annealed films and casg and can are, respectively, the corresponding values of the lattice constant c. The
expected values of the initial decrease in the extraordinary
refractive indices due to the observed lattice contraction
c f in the two films according to Eq. (3) nef l are given
in Table III, along with the corresponding experimental values nef (Fig. 3). The calculated values are found to be
much higher than the experimentally observed decrease in
nef for the same change in lattice constant c f . This deviation clearly indicates the contribution of increase in packing
density during annealing on the refractive indices, in addition
to the role of lattice contraction. The values of packing density p of ZnO films were determined from the experimental
values of the refractive indices by Gupta and Mansingh4 using various formulae. The best results were obtained after
assuming cylindrical shape of crystallites of the films using
the following equation:7
n f p =

1 pnv4 + 1 + pnv2nb2
1 + pnv2 + 1 pnb2

after incorporating the contribution of lattice variation toward the change in refractive index [from Eq. (2)] and the
modified relation is
n f = n f p + n f l nb
=

1 pnv4 + 1 + pnv2nb2
1 + pnv2 + 1 pnb2

5 n b2 1
c f cb,
2 n bc b
5

where the first and second terms in Eq. (5) represent the
contribution to the refractive index from the packing density
and the lattice constant c changes, respectively. Accordingly,
the refractive index of the film would be found to increase or
decrease as compared to the bulk value, depending on which
of these two effects dominates. The packing density of the
as-grown and annealed ZnO films were determined from the
experimental values of nef and c f as well as nof and c f , using
Eq. (5). The estimated values of packing density determined
from nef and nof for the same film were found to be very
close to each other with a standard deviation ranging from
0.0002 to 0.001. The average of these two values of packing density is plotted in Fig. 5 as a function of annealing time
for the films S1 and S2. The values of the packing density of
these films as determined from Eq. (4), without considering
the effect of the lattice, are also shown in the figure for
comparison. It may be noted that the variation of the packing
density, determined from Eq. (5) and Eq. (4) with annealing
time, shows different trends. The estimated values of packing
density of as-grown films using Eq. (5) are considerably
lower than those determined using Eq. (4). The maximum
increase in packing density according to Eq. (5) was ob-

where nv is the refractive index of voids =1 and the packing density of bulk is taken as one. The influence of lattice
contraction was not considered.
Considering the simultaneous role of factors p and c f in
influencing the refractive index, Eq. (4) could be modified

FIG. 5. Estimated values of packing density of ZnO films p, deposited by

rf magnetron sputtering with deposition conditions as in Table I and after
annealing at 380 C in air at different times, using Eq. (5) and experimental
values of c f , nef , and nof (Fig. 3 and 4). The corresponding values estimated
using Eq. (4) (dashed lines) are also given for comparison.

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3138

Mehan et al.

J. Appl. Phys., Vol. 96, No. 6, 15 September 2004

TABLE IV. Contribution to nef nb from nef l nb [Eq. (2)] and nef p nb [Eq. (4)] for as-grown and
annealed ZnO films. Values of c f cb for the films are given
Film S1

Film S2

Annealing
time (h)

nef p nb

nef l nb

c f cb

nef p nb

nef l nb

c f cb

0
0.5
1
2
3

0.0664
...
0.0307
0.0186
0.0174

0.0452
...
0.0017
0.0078
0.0089

0.0625
...
0.0023
0.0108
0.0123

0.0396
0.0305
0.016
0.0117
...

0.0134
0.0028
0.0078
0.0089
...

0.0185
0.0038
0.0108
0.0123
...

served in the first hour of annealing, after which it showed a

saturation tendency to a value close to the bulk value for
both the films. The packing density values of the films estimated without considering the effect of lattice [i.e., from Eq.
(4)] showed an initial decrease on annealing. It is noted that
the value of p for the as-grown film deposited in O2 - Ar
composition 80:20 (film S1) as estimated from Eq. (5), is
much lower than the corresponding value for the film deposited in O2 - Ar ratio 60:40 (film S2). However, the corresponding values of p for both the films S1 and S2 estimated
using Eq. (4), are reasonably close to each other. Thus, the
packing density of the as-deposited films, determined after
taking the effect of the lattice into account, depends significantly on the sputtering gas ambient in which the film is
deposited, which is expected. It may be noted in this context
that the crystalline orientation of the as-grown film S2 is
much better than that of the as-grown film S1, and the grain
size of the film S2434 is also much greater than that of
film S1189 . Because the lattice constant of the as-grown
film S1 is much more elongated as compared to bulk value
than that of film S2, the positive contribution to nef nb [Eq.
(5)] due to lattice expansion, i.e., nef l nb) is much
greater (more than three times) in case of the film S1, as
shown in Table IV. However, the negative contribution due
to the lower packing density i.e., nef p nb, is also more
pronounced in the as-grown film S1 as compared to that in
film S2. This explains why the extraordinary refractive indices of as-deposited films S1 and S2 are very close to each
other (Fig. 3) despite the large differences in the structural
properties of these films, viz., lattice constant c f and packing
density (Fig. 4 and 5). As noted from the table, both the
lattice constant c f and the packing density approach the respective bulk values on annealing, and after 1 h nef l nb
gives a negative contribution to the refractive index.
Figure 6 shows the packing density of ZnO films deposited by rf diode sputtering using an oxide target and annealed
at different temperatures,4 estimated using Eq. (5) and the
corresponding values obtained using Eq. (4) from the reported values of refractive indices of these films (determined
from UV-VIS spectroscopy).4 The proximity of these values
up to an annealing temperature of 600 C indicates that the
effect of lattice constant c on changes in the refractive index
is less significant for these films, as compared to that for the
rf magnetron-sputtered films studied in the present case. The
effect of change in the packing density was found to dominate in these films, which may be attributed to the fact that

the deviation of p from the bulk value is more pronounced

than that of c f in these as-deposited rf diode-sputtered films.4
V. CONCLUSIONS

The observed initial decrease and subsequent increase in

the refractive indices of rf magnetron-sputtered ZnO films
with the annealing time at a fixed-annealing temperature
380 C in air indicate that both the packing density and the
lattice constant c influence the refractive index of ZnO films.
A relation is proposed to estimate the packing density of zinc
oxide films when the lattice constant c is different from the
bulk value. The estimated values of the packing density of
the as-grown and annealed rf magnetron-sputtered ZnO films
from refractive indices show the expected behavior of an
initial rapid increase with annealing time and a saturation
tendency at a higher annealing time, only when the influence
of the changes in lattice constant c on the refractive index are
taken into consideration. After this modification, the packing
density of the as-deposited ZnO films is found, as anticipated, to depend on the sputtering gas ambient.
ACKNOWLEDGMENTS

The authors are grateful to the University Grants Commission (UGC) for financial assistance.
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FIG. 6. Packing density of rf diode-sputtered ZnO films p in an as-grown

condition and after annealing at different temperatures in air from Eq. (5),
using experimental values of refractive indices (Ref. [4]). The corresponding
values estimated from Eq. (4) (dashed lines) are also given for comparison.

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