Optics Communications 225 (2003) 341–348

www.elsevier.com/locate/optcom

Refractive index and thickness determination

of thin-films using LloydÕs interferometer
A.A. Hamza a, M.A. Mabrouk b, W.A. Ramadan b,*
, A.M. Emara b

a
Physics Department, Faculty of Science, Mansoura University, Mansoura, Egypt
b
Physics Department, Faculty of Science (Damietta), Mansoura University, Damietta, Egypt
Received 15 May 2003; received in revised form 30 July 2003; accepted 2 August 2003

Abstract

Determination of the refractive index and the thickness of thin-films using light interference have been presented.
This has been done, for the first time, with the use of LloydÕs interferometer. The mean idea is based on using the sample
in two different positions in the same interferometer. The method has been applied for four different samples with
different thickness. The thickness is measured using a reflection regime in a separate step. In case of determining both of
refractive index and thickness of the thin films, the needed data have been obtained directly from a comparison between
two interference fields in the same interferogram for each case. In this way we avoid mistakes that could be produced
from the direct experimental measurements. The method with its simplicity, in experimental mounting and mathe-
matical interpretation, can offer quite accurate results. An investigation of the uncertainty in the measured values
demonstrates that, for the measured thickness we have a tolerance of 3% and for refractive index the tolerance is

0.002, which is the reasonable for two-beam interference systems.

2003 Elsevier B.V. All rights reserved.

PACS: 07.60.Ly; 42.25.Hz; 78.66.Qn; 78.20.Ci

Keywords: Interference; Thin films; Refractive index; Thickness

1. Introduction optical properties of the thin film, especially the

Thin films are very important in many applica-
tions such as integrated optical circuits, polarizers,
low-pass filter, beam splitter and antireflection film.
For these applications, it is important to know the
* fractive indices and thickness simultaneously. Chiu
Corresponding author. Tel.: +20-57-403866; fax: +20-57-
403868.
E-mail address: wramadan_eg@yahoo.com (W.A. Rama-
dan).
refractive index and the thickness. Many attempts
were made to determine these two parameters ac-
curately. Lee et al. [1] measured the refractive indi-
ces when using light vibrating parallel and
perpendicular to the film surface from the reflec-
tivity. This technique gives both values of the re-
et al. [2] used another method for measuring the
refractive index. Beginning with measuring phase
difference between parallel and perpendicular

0030-4018/$ - see front matter
2003 Elsevier B.V. All rights reserved.
doi:10.1016/j.optcom.2003.08.003
342 A.A. Hamza et al. / Optics Communications 225 (2003) 341–348
polarizations of the light used at the total internal
reflection, this was done by the heterodyne inter-
ferometric technique, then it is substituted into
FresenelÕs equations, and the refractive index of the
test thin film is obtained. The measurable range of
this technique is limited by the refractive index of the
prism. To expand the measurable range it is better to
use a prism with a high refractive index.
Zheng and Kikuchi [3] measured refractive in-
dex and the extinction coefficient of a weakly ab-
sorbing thin film using analytical method, which is
based on measurements of the reflectance extreme
and corresponding transmittance of the film at
normal incidence.
One of the most important techniques is
ellipsometry, Jenkins [4]. It is a technique that has
been studied for several centuries. However, it has
recently found much favor in the non-destructive
characterization of solids, particularly semicon-
ductors. The modern era of measurement of the
ellipticity of light arguably began in 1945 with the
work of Rothen [5]. He devised a simple form of
rotating analyzer ellipsometer, consisting of a light
source, polarizer, sample and an analyzer in the
form of a quarter-wave plate and another pola-
rizer. By rotating the analyzer, it was possible to
determine the ellipticity of the light reflected from
the surface of the sample. But in this technique the
refractive index is given via the reflection mea-
surement, which make it quite complicated.
Many authors used reflectance dependent
techniques [6,7] to determine the thickness of a
thin film. Davazoglou [8] used a transmission
technique to study the optical dispersion and film
thickness of a semiconductor layer.
Interference dependent techniques [9–12] are
used as well to measure the thin-film thickness.
Hernandez et al. [11] used Michelson interferome-
ter to measure the film thickness. They replaced one
of the MichelsonÕs interferometer mirrors by a
substrate containing partially (as step) the film.
Although this method gives good results at certain
wavelengths, the measured thickness depends on
the wavelength used, and the obtained fringes have
a poor resolution. Liu et al. [12] used a non-contact,
non-destructive and simple method for measuring
the thickness, refractive index and extinction coef-
ficient of a dip coated film by using p-polarized laser
beams. In this method, the oblique sample is illu-
minated with a p-polarized laser beam to measure
the intensity ratio of the two reflected beams, from
the front and back surfaces after receiving them
with a detector, versus the angle of incidence. The
parameters of the film were obtained by means of
data fitting.
Recently, LloydÕs interferometer has been used
by Bertolotti and co-workers [13] to determine di-
rectly the refractive index profile of a planar graded
index waveguides. Moreover, the same group
[14,15] has used this technique, for the first time, to
detect experimentally the birefringence in the used
Kþ –Naþ ion exchange samples. Here, we underline
that LloydÕs interference technique was applied on
graded index samples. For step index planar wave-
guide, the problem was not solved yet. In the present
work, we provide the first trial to measure the re-
fractive index and thickness of polymeric thin films
using LloydÕs interference. This interference system
can offer some advantage in comparison with the
previously nominated ones. In case of thickness
investigation, the measurement is reflection depen-
dent, so, the transparency and the refractive index of
the investigated film do not affect our measure-
ments. Moreover, due to use of the light source as a
line parallel to the sample surface, the variation of
the film thickness (on macro-scale) can be detected.
2. Theory
In this work the substrate carrying the film will
be hold in two different positions. Position A (de-
scribed in Fig. 1); in which the sample itself is used
instead of the mirror in LloydÕs interferometer. In
this position the thickness of the thin film can be
determined. Position B (described in Fig. 3); in
which the sample is inserted in the beam path to
cause a shift in the observed fringes. The refractive
index of the thin film can be determined measuring
that shift.
2.1. Position A
Interference takes place in LloydÕs mirror be-
tween the direct and reflected rays on the mirror.
The substrate containing the film is used as a
 A.A. Hamza et al. / Optics Communications 225 (2003) 341–348
Fig. 1. The experimental set-up describing position A. The
sample is used as a LloydÕs mirror.
LloydÕs mirror as shown in Fig. 1, which shows the
set-up representing LloydÕs interferometer used to
determine the film thickness. The line source sends
light on the film and substrate surfaces at the same
time. Two field patterns are produced. The first is
due to reflection on the substrate only and the
second is due to reflection on the film surface as
shown in Fig. 2(a). The optical path difference
producing such fringes can be found considering
the theoretical interpretation mentioned in [16].
Fig. 2. A schematic diagram representing LloydÕs two-beam
interference. (a) The substrate with and without the thin film
works as two mirrors and shows different optical paths. (b) A
schematic diagram representing the produced fringe patterns.
343
According to this theory, we have to consider that
the distance between the two sources d is very
small compared with the distance between the
source and the screen D. In our case we are satis-
fying this condition (typical values are d  80 lm
and D  25  104 lm). Also, according to the used
set-up (see Fig. 1), the incidence angles on the re-
flected surfaces are found to be in the range of
84.8–89.8, which give high value of reflected light
intensity. In this case the contribution of phase
change, due to the reflection on the thin film, is
minimized and could be neglected [16].
On the screen, two pattern fields can be ob-
served; substrate fringes field and film with
substrate fringes field, as shown in Fig. 2(b). The
first pattern is characterized by a small fringe
width b1 , while the other has a wider fringe
width b2 . This is because the vertical distance
between the source and the reflecting surface, in
case of substrate only is d, and is greater than
that between the source and the film surface
ðd  tÞ; t is the thickness of the film. The ratio
between b1 and b2 can be given by
b1 d  t
¼ : ð1Þ
b2 d
This ratio can be calculated from the micro-
interferograms because the zero-order fringes of
both patterns coincide with each other. If x is the
distance between the zero-order fringes of the two
patterns and any point on the micro-interferogram
as shown in Fig. 2(b), the ratio between the fringes
width is given by
b1 m  a
¼ ; ð2Þ
b2 m
where a is the fractional number of fringe order.
It can be expressed as Dh=h at the mentioned dis-
tance x or at a certain order m, where h is the in-
terfering spacing of the substrate and Dh is the shift
due to the film. From Eqs. (1) and (2), the thickness
can be expressed in the following form:
ad
t¼ : ð3Þ
m
This equation can be used to determine a wide
range of thin films thickness regardless to their
material transparency and refractive index.
344 A.A. Hamza et al. / Optics Communications 225 (2003) 341–348

2.2. Position B In the path of this parallel beam, we put a rect-

In this position, we used the parallel beam of
light coming from the collimating lens. When this
beam is incident on the cylindrical lens, half of it is
emerging from the lens to reach the screen directly
while the other half is incident on a mirror to be
reflected toward the screen. In this case two-beam
normal LloydÕs interference can be observed, the
interference fringes are in the form of parallel lines,
which are parallel to the line source and are
characterized by good visibility and equal fringe
width.
Fig. 3. The experimental set-up describing position B. The
sample is inserted in the path of the parallel beam to cause a
shift in normal LloydÕs fringes.
angular optical cell perpendicular to the optical axis
and containing a suitable matching liquid, see
Fig. 3. The liquid is chosen to make the path length
difference between the light passing through the
substrate (Fig. 4(b)) and the film-substrate
(Fig. 4(c)) is not more than one wavelength of the
light used. So, we can avoid the doubt in defining
the fringe shift order. The sample has been im-
mersed in this liquid and is adjusted to make its
boarder tangent to the optical axis and the edge of
the thin film dividing the half of light spot (see
Fig. 4(a)). In this case one of the interfering beams
passes through the liquid only, reflected beam. The
second beam, part of it passes through the substrate
while the other part passes through the substrate
and the film together. These beams will constitute
the direct beam, which interfere with the reflected
one. Due to this optical configuration, we will get
on the screen two patterns of interference. They
have the same fringe width but one of these patterns
is suffering a shift with respect to the other. Now
let us follow the optical path length difference for
each case.
In the first case, we have a reflected beam tra-
versing only the liquid and the direct beam tra-
versing the substrate material, see Fig. 4(b). So the
optical path difference can be given by
D 1 ¼ j ns  nL j T s ; ð4Þ

Fig. 4. This figure illustrate, how the edge of the sample divided the laser parallel spot into two half and the light passing through the
sample is divided by the edge of the thin film into two parts (a). The light paths in case of substrate and liquid interference and in case
of substrate with thin-film and liquid interference are shown in (b) and (c), respectively.
 A.A. Hamza et al. / Optics Communications 225 (2003) 341–348 345

where ns and nL are the substrate the liquid re- 3. Experimental set-up and results
fractive indices, respectively. Ts is the substrate
thickness. In this set-up a laser beam passes through a
In the second case, the reflected beam traverses spatial filter and a collimating lens to get a wide
only the liquid and the direct beam will traverse spot of a parallel beam. A cylindrical lens fo-
the substrate and the film materials, see Fig. 4(c). cuses this parallel beam on a line, which is used
So the optical path difference can be written as as a line source. The line source is located in
front of the sample (position A) or a mirror
D2 ¼ jns  nL j Ts þ jnf  nL j t; ð5Þ
(position B). In position A, the specular face of
where nf and t are the refractive index and the the substrate and the film is used to do the
thickness of the film, respectively. mirror job in LloydÕs interferometer, Fig. 1.
From Eqs. (4) and (5) one can notice that the Adjusting the position of the sample, one can
presence of the substrate or of the substrate with observe the formation of the fringes shown in
the film, in the path of one of the interfering Figs. 5(a)–(d). In position B, an optical cell
beams, will cause a constant change in the phase. containing a matching liquid is inserted perpen-
In other words, all the fringes will suffer a constant dicular in the path of the parallel beam after the
shift in their order. This shift is directly propor- collimating lens, Fig. 3. The substrate carrying
tional to the values of D1 and D2 .
To determine directly the film refractive index
let us subtract Eq. (4) from Eq. (5)
Df ¼ D2  D1 ¼ jnf  nL j t: ð6Þ
This simply means that the displacement between
the two obtained patterns is coming only from the
presence of the thin film. Thus the problem of
determining the refractive index of the film is re-
duced to determine experimentally the path dif-
ference Df . The path difference can be recovered
from the interferogram, considering that the dis-
tance between any successive bright or dark fringes
on the screen is equivalent to the path difference
between the interference beams, which equal to
one wavelength of the light used. So, Df can be
calculated from the relation

Dhb
Df ¼ k ; ð7Þ
hb
where hb is the interfering spacing and Dhb is the
shifted distance of the film fringes.
From Eqs. (6) and (7) we can get the refractive
index nf as
k Dhb
nf ¼ nL
: ð8Þ
t hb
Fig. 5. The LloydÕs interferograms obtained when holding the
The positive or the negative sign will be chosen
sample in position A. The interferograms (a)–(c) show the co-
according to the direction of the shift. When the incidence between the double-field fringes for samples I–III,
shift is toward or far from the optical axis the sign respectively. In interferogram (d) the film thickness of sample
will be negative or positive, respectively. IV is too thin to provide fringes to coincide.
346 A.A. Hamza et al. / Optics Communications 225 (2003) 341–348
the thin film is immersed in the liquid perpen-
dicular to the parallel beam. The sample has
been adjusted to accommodate the position il-
lustrated in Fig. 4. Due to the optical path dif-
ference between the liquid and the film a shift
can be noticed in the straight-line fringes, Figs.
6(a)–(d). The interferograms obtained from these
configurations have been recorded in a cut-film
and scanned to a computer. The parameters
needed for the calculation a, hb and Dhb has
been determined using a computer image pro-
gram. The value of d has been measured directly
using the micrometer of the precise translation
stage with the observation of the light diffraction
from the sample board. The wavelength of the
light used was 632.8 nm and the liquid used has
a refractive index of 1.462.
Thin films of different thickness were prepared
from the same polymer material on a flat sub-
strate. The sample was adjusted in position A
shown in Fig. 1. Two interference fringe fields
are constructed in the same pattern. Fig. 5 shows
Fig. 6. Interferograms produced by LloydÕs interferometer with
sample in position B. The interferograms, shown in (a)–(d), are
used to determine the film refractive index of the samples I–IV,
respectively.
the double-field interference patterns for four
samples (labeled I, II, III and IV) of different
thickness. The LloydÕs interference pattern of the
sample-I is shown in Fig. 5(a). Because the film
has a relatively thick value, first coincidence
between the fringes in the double-field takes
place at the sixth and the seventh fringes. In this
image the measured value of d is 61:3 lm. De-
creasing the film thickness, coincidence occurs at
higher interference orders. For sample-II, the
pattern is shown in Fig. 5(b). Coincidence takes
place at the fringes of orders 11 and 12. For
sample-III, with smaller film thickness, coinci-
dence happens at the fringes of orders 22 and 23
as shown in Fig. 5(c). In these cases, the frac-
tional order a is equal to one and m (order
number) takes the values 7, 12 and 23, respec-
tively. Also, the measured values of d used with
samples I, II and III were 61.3, 66.3 and 81.3
lm, respectively. The fourth sample has the
smallest thickness, no coincidence can be ob-
served but a small shift between the fringes can
be seen at higher interference orders as shown in
Fig. 5(d). Herein, the value of a is dependent on
the value of m. So different mÕs and their core-
spondent values of a have been taken to verify
the measured thickness and substituted in Eq.
(3). Table 1 shows the measured values of the
film thickness for different m and a on the in-
terferogram, or we can say at different locations
on sample surface. These values are found to
converge around an average value regardless to
the used order.
To determine the refractive index, the sample
has been put in position B, Fig. 3. The obtained
interferograms are shown in Figs. 6(a)–(d). One
can notice that the fringes shift increases with in-
creasing the sample thickness. The magnitude of
the shift is a function of the refractive index of the
liquid used. It is expected that for small thickness,
the matching liquid could not be used any more,
when the difference on the optical path between
the light passing through the film material and the
air does not exceed one order or k. Using Eq. (8),
the refractive index of the samples has been de-
termined. Table 2 shows the thickness and the re-
fractive indices obtained for the different samples.
Here, we underline that the thickness of the sample
 A.A. Hamza et al. / Optics Communications 225 (2003) 341–348 347

Table 1
The determined thickness t at different order m and their corespondent a
Thickness of sample-I Thickness of sample-II Thickness of sample-III Thickness of sample-IV
(lm) (lm) (lm) (lm)
8.75
0.4 5.52
0.2 3.53
0.1 0.91
0.03
8.70
0.4 5.34
0.2 3.45
0.1 0.92
0.03
8.63
0.4 5.33
0.2 3.55
0.1 0.88
0.03
8.98
0.4 5.36
0.2 3.49
0.1 0.89
0.03
8.63
0.4 5.28
0.2 3.42
0.1 0.88
0.03
– 5.33
0.2 3.50
0.1 0.87
0.03
– 5.57
0.2 3.47
0.1 0.88
0.03
8.74
0.4 5.39
0.2 3.49
0.1 0.89
0.03
The average values are listed at the end raw.

Table 2
Refractive index for different samples; the used values of thickness, interfringe spacing hb , the shift values Dhb and the accuracy are
shown
Sample t (lm) hb (mm) Dhb (mm) nf
g
I 8.74 11.0 9.21 1.523 2.4  103
II 5.39 8.50 4.44 1.523 2.3  103
III 3.49 9.00 3.00 1.522 1.8  103
IV 0.89 8.23 0.72 1.524 1.9  103

has been determined in a separate step. This is the 4. Conclusion

mean difference between the presented interference
method and the most of other interference tech- This study demonstrates the capability of
niques. LloydÕs interferometer for investigating thin films
The accuracy c, of the measured thickness can with high efficiency. The method has been applied
be determined using the following expression [11]: to determine the thickness and the refractive in-
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
 2  2 dex of four thin-film samples. The method was
ot ot sensitive to determine thickness up to 0.89 lm
c¼
ðDaÞ2 þ ðDd Þ2 ; ð9Þ
oa od with an accuracy of 3% of the measured value.
Due to the good determination of the thickness
where Da and Dd are the error in the experimental
independently of the refractive index, the deter-
measurement of the values a and d, respectively.
mination of the refractive index was quite accu-
The error in determining the refractive index is
rate (
0.002).
propagating due to the uncertainty of defining Dab
Due to the simplicity of experimental prepara-
and the error in determining t. So, this error could
tion of the set-up and of the mathematical inter-
be evaluated from the following equation:
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi pretation, the method result very promising for the
 2  2 following reasons:
onf 2 onf 2
g¼
ðDab Þ þ ðDtÞ ; ð10Þ • The method is reflection dependent and does
oab ot
not depend on the transparency of the film ma-
where Dab ¼ DðDhb =hb Þ is the experimental error terial, so the thickness of both opaque and
in determining ðDhb =hb Þ. The partial derivatives in transparent samples can be measured.
Eqs. (9) and (10) represent the error accumulated • Few parameters must be measured directly
from the dependence of the calculated parameter (t from the interferograms. This means increasing
and nf ) on the experimentally measured values (a, the speed and reducing the error in the measure-
d and ab ). ments.
348 A.A. Hamza et al. / Optics Communications 225 (2003) 341–348
• The method can be used to measure a wide
range of thickness. One can notice from the de-
scribed results that we are able to determine
thin film thickness ranging from fractions of mi-
crometers up to 9 lm. This range is suitable for
studying the step index planar waveguides.
• In case of position B, adapted to measure the
refractive index, one cannot use an immersion
liquid if the thickness of the sample is less than
a certain value that depends on the wavelength
of the light used. This means a complete deter-
mination of the film parameter in a non-
destructive, non-contacting and direct way can
be done.
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