Analysis of errors in thin-film optical parameters derived

from spectrophotometric measurements

at normal light incidence

Ivan Konstantinov, Tzewatanka Babeva, and Snejana Kitova

A comparative analysis is made of the errors in deriving the optical parameters ~n, refractive index; k,
absorption coefficient; d, film thickness! of thin films from spectrophotometric measurements at normal
light incidence. The errors in determining n, k, and d by the ~TRf Rb!, ~TRf Rm!, ~TRb Rm!, ~TRf !, ~TRm!,
and T~k 5 0! methods are compared. It is shown that they are applicable to optical constants of thin
films in the n . 1.5, k , 4.5, and dyl 5 ~0.02–0.3! range, and their combinations make possible the
determination of n and k to an accuracy of better than 64%. To derive the optical constants in a wide
spectral range with high accuracy and isolate the correct physical solutions reliably, one should apply all
methods, using the relevant solutions with the lowest errors, as shown in this research, when determin-
ing the optical constants of As2S3 and Sb2Se3 films. © 1998 Optical Society of America
OCIS codes: 120.0120, 120.4530, 120.6200, 310.0310, 310.6860.

1. Introduction cability, depending on the investigated object and the

Recently, we published algebraic methods1–3 for cal-
culating the optical parameters ~n, refractive index;
k, absorption coefficient; d, film thickness! of thin
films from combinations of three measured photomet-
ric quantities at normal light incidence—the ~TRf Rb!,
~TRf Rm!, ~TRb Rm!, and T~k 5 0! method in the non-
absorbing spectral range ~k 5 0!. Subscripts f, b
denote reflection R from the side of the thin film and
the substrate, and m is the reflection of the film onto
an opaque metal substrate. Now, analyzing the er-
rors of the corresponding methods, we determine
their acceptable fields of applicability, limited by the
accuracy of the photometric quantity measurement.
Generally, we cannot expect the accuracy of TRR
methods to be superior to that of TR methods. Since
each method has different precision, depending on
the values of n, k, and dyl, we should expect that the
high-accuracy regions of the methods will be differ-
ent, and hence every method will have its own appli-
The authors are with the Central Laboratory of Photoprocesses,
Bulgarian Academy of Sciences, Academy G. Bonchev str., bl. 109,
Sofia 1113, Bulgaria.
Received 2 October 1997; revised manuscript received 2 March
1998.
0003-6935y98y194260-08$15.00y0
© 1998 Optical Society of America
spectral range.
A major advantage of the TRR methods is the pos-
sibility of determining the film thickness, thus ~1!
eliminating additional measurements, i.e., additional
instrumentation and appropriate experimental
skills, and ~2! giving an objective criterion for isolat-
ing the correct solutions.
Methods of calculating the errors in n, k, and d,
depending on the accuracy of the measured quanti-
ties, are known.4 – 6 Most of the authors have, how-
ever, applied the error assessment only for particular
determinations or in a specific spectral range.4 – 6
Only Hansen7 has attempted a comparison of the
accuracy of the different methods but only on the
basis of concrete values of n, k, and dyl. The con-
clusions are, however, not always correct for other
values of n, k, and dyl because of their quite different
errors.
In the present research we compare the maximum
errors in the calculation of n, k, and d by the TRR
methods with those of the TR and T~k 5 0! methods
in broad ranges of n, k, and dyl. Using concrete
experimental examples, we prove the necessity of
combining the methods to determine more precisely
the optical constants in a wide spectral range.
2. Calculation of Errors in n, k, and d
Calculation of the absolute andyor relative maximum
error in determining n, k, and d arising from small

4260 APPLIED OPTICS y Vol. 37, No. 19 y 1 July 1998

experimental inaccuracies in the measured quanti- Thus we can use Eq. ~4! to calculate the derivatives
ties and in the substrate optical constants is a famil- in Eqs. ~1!, using the easy calculated derivatives in
iar procedure.4 – 6 Eqs. ~2! or Eq. ~3!.
In the TRRm methods, where R is either Rf or Rb, The relative maximum errors, for example, Dnyn,
the absolute maximum errors are functions of the are determined by
type Dn, Dk, and Dd 5 f ~DT, DR, DRm, Dns, Dnm,
Dkm!, where the symbols in parentheses are the un- Dn DT DR DRm Dns
certainties in the measured quantities. Since error 5 uE11u 1 uE21u 1 uE31u 1 uE41u
n T R Rm ns
Dl in wavelength is negligibly small ~Dl ' 0!, abso-
lute errors Dn, Dk, and Dd can be expressed as Dnm Dkm
1 uE51u 1 uE61u , (5)

UU U U U U U U
nm km
]n ]n ]n ]n
Dn 5 DT 1 DR 1 DRm 1 Dns
]T ]R ]Rm ]ns where the coefficients Eij are given in the error

U U U U
matrix @Eq. ~6!#, similar to Hansen’s matrix7:
]n ]n

5 6
S D SD F G
1 Dnm 1 Dkm,
]nm ]km T ]n T ]k T ]~dyl!

Dk 5 UU
]k
DT 1U U
]k
DR 1
]k
U U
DRm 1
]k
U U
Dns
n ]T k ]T ~dyl! ]T

1
]T

U ]k
]R

U U
Dnm 1
]k
]Rm

U
Dkm,
]ns
S
R ]n
n ]R
D SD R ]k
k ]R
R
~dyl!F]~dyl!
]R G
Dd 5
]d
UU
]nm

DT 1
]d
U U
]km

DR 1
]d
U U
DRm 1
]d
Dns U U S
Rm ]n
n ]Rm
D S D Rm ]k
k ]Rm F
Rm ]~dyl!
~dyl! ]Rm G
S D S D F G
]T ]R ]Rm ]ns E5 . (6)
ns ]n ns ]k ns ]~dyl!
1U ]d
U U
Dnm 1
]d
U
Dkm. (1) n ]ns k ]ns ~dyl! ]ns

S D S D F G
]nm ]km
nm ]n nm ]k nm ]~dyl!
Since the partial derivatives cannot be evaluated n ]nm k ]nm ~dyl! ]nm

S D S D F G
numerically, they must be expressed by derivatives
that can be calculated. For this purpose, simple lin- km ]n km ]k km ]~dyl!
ear expressions are used, which for the TRRm meth- n ]km k ]km ~dyl! ]km
ods have the form

DT 5 SD SD
]T
]n
Dn 1
]T
]k
Dk 1
]T
]d
SD S D
Dd 1
]T
]ns
Dns,
In a similar way, Dkyk and Ddyd are calculated by
the corresponding columns of error matrix ~6!. We
mentioned above that Dl is negligibly small, so the
DR 5 SD SD
]R
]n
Dn 1
]R
]k
Dk 1
]R
]d
SD S D
Dd 1
]R
]ns
Dns,
relative error Ddyd is equal to D~dyl!y~dyl!.
Similarly, for the T~k 5 0! method,

DRm 5 S D S D
]Rm
]n
Dn 1
]Rm
]k
Dk 1 S D
]Rm
]d
Dd DT 5 SD SD S D
]T
]n
Dn 1
]T
]d
Dd 1
]T
]ns
Dns. (7)

1S D S
]Rm
]nm
Dnm 1
]Rm
]km
D
Dkm. (2) Hence Dn is

Dn 5 uE1uDT 1 uE2uDd 1 uE3uDns,

YS D S DYS D
Using a more compact matrix expression, we write
Eqs. ~2! as ]T ]T ]T
E1 5 1 E2 5

S D SD S D
, ,
]n ]d ]n
DT Dn Dns
DR 5 M1 p Dk 1 M2 p Dnm .
DRm Dd Dkm
(3) E3 5 S DYS D
]T
]ns
]T
]n
. (8)

The solution is obtained by matrix multiplication The relative error is

with the inverse matrix M121:

U U U U U U
SD S D S D
Dn T DT d Dd ns Dns
Dn DT Dns 5 E1 1 E2 1 E3 . (9)
n n T n d n ns
Dk 5 u~M1!21u p DR 1 u~M1!21 p ~M2!u p Dnm .
Dd DRm Dkm The values of T and R of the thin film are calculated
(4) from T and R, the transmission and the reflection of

1 July 1998 y Vol. 37, No. 19 y APPLIED OPTICS 4261

the sample, which include the effect of the back sur- @Eqs. ~12!# with coefficients A 5 10.43 and B 5 319.93,
face of the substrate, by8 whereas the values of km are

T~Rs 2 1! km 5 1y~ A 1 Bl2 1 Cl3!, A 5 5.86,

T5 ,
1 1 Rb Rs 2 2Rs B 5 22.3 3 10 ,24
C 5 5.2 3 1027. (13)

Rf 5 Rf 2
T Rs 2

1 1 Rb Rs 2 2Rs
, Rs 5 S D
ns 2 1
ns 1 1
,
2

The numeric calculations are performed for values

of ns, nm, and km at l 5 550 nm. Similar calcula-
Rb 2 Rs tions with corresponding values at different l within
Rb 5 , (10) the 400 –1000-nm range do not substantially change
1 1 Rb Rs 2 2Rs
the results discussed in Subsection 3.A.
This analysis enables us to draw only general con-
where ns is the refractive index of the nonabsorbing
clusions about the applicability of the methods used.
substrate.
Owing to the great number of quantities governing
DT and DR in Eq. ~5! @with respect to Eqs. ~1!–~4!#
accuracy, it is very difficult to present results from a
are then obtained from
complete analysis, enabling the researcher to choose

U U U U U U
the most suitable method in a given spectral range,
]T ]T ]T depending on the accuracy of the measured photo-
DT 5 DT 1 DRb 1 DRs,
]T ]Rb ]Rs metric quantities. The practical approach is to eval-

U U U U U U U U
uate the error in each set of the obtained n, k, and d
]Rf ]Rf ]Rf ]Rf of the investigated thin film and to compare directly
DRf 5 DT 1 DRf 1 DRb 1 DRs,
]T ]Rf ]Rb ]Rs the results from the various methods. This is illus-

U U U U
]Rb ]Rb
DRb 5 DRb 1 DRs.
]Rb ]Rs
3. Maximum Errors in Photometric Methods for
Normal Light Incidence
In the following considerations we present a sche-
matic picture of the errors in the optical constants
and the thin-film thickness as dependent on the val-
ues of n, k, and dyl. The experimental inaccuracies
assumed in the spectrophotometric quantities are
DT 5 60.001 and DR 5 60.005, and the errors in
the refractive indices of the two substrates are
Dns 5 60.015, Dnm 5 60.03, and Dkm 5 60.02.
Corresponding inaccuracies DT and DR are calcu-
lated by Eqs. ~11!. The values of T, Rf, and Rm are
calculated by Fresnel equations ~Ref. 8, pp. 6 – 8!, and
the maximum errors are calculated by the equations
in Section 2. Because nonabsorbing substrate BK7
glass is assumed, ns is calculated by the dispersion
formula of Sellmeier ~Ref. 8, p. 134!:
trated by the following examples.
(11)
A. Maximum Relative Errors in TRR Methods
In TRR methods three different combinations be-
tween the photometric quantities are possible—
~TRf Rb!, ~TRf Rm!, ~TRb Rm!. The first combination
is the least applicable, since it is unusable for
the films in the spectral range around and beyond
their absorption edge,1 where Rf 5 Rb. Besides, the
analysis performed showed that the errors in this
combination are substantially higher than those in
the two other combinations. Because in the two
combinations with Rm the errors differ negligibly, in
the following we present the results on the ~TRf Rm!
method only.
1. Assessment of the Error Matrix Terms
According to Hansen,7 the method for determining
the optical constants is excellent if the error matrix
terms @Eq. ~6!# are near unity or less. A value of
unity for each element of the matrix @Eq. ~6!# means
that optical parameters n, k, and d are determined to

F G 1y2 the same accuracy as the corresponding measured

A quantities T, Rf, Rm, ns, nm, and km.
ns 5 1 1 , A 5 1.26, B 5 98.94.
1 2 ~Byl!2
The methods including Rm are made difficult by the
necessity of using a suitable metal film with known
nm and km. Our experience showed that carefully
polished Si wafers are appropriate. They are easily
accessible, and if their surface is cleaned by the
adopted procedure,9 they reproduce excellently the
values of the reflectance calculated from the high-
accuracy optical constants.10 This eliminates the
necessity of depositing an opaque metal film with
reproducible optical constants, as well as their deter-
mination, which is not always feasible by spectropho-
tometric methods. The nm values of the Si
substrate10 are evaluated by the dispersion formula
(12)
Figure 1 displays the regions in the n–k plane,
defined by the terms of the first column of the error
matrix ~6! with values of #1, dictating the error in n
at dyl 5 0.1. It is evident that the region in which
all terms are #1 is limited for n . 1.5 and k , 1.5.
The terms T, ns, nm, and especially km make a
smaller contribution to the error in the determination
of n. Note that the km terms have values smaller
than 0.1 over almost the whole n–k plane. Only the
contours with a value of 0.1 are drawn in Fig. 1~b!.
Taking into account that the measurement of the film
transmittance is much more accurate than that of the
reflectance, as well as the high accuracy of ns, nm, and
km, obviously the regions of good accuracy are gov-
erned by the terms of the reflectance. Besides, the

4262 APPLIED OPTICS y Vol. 37, No. 19 y 1 July 1998


Fig. 1. Regions in the n–k plane, defined by terms of the first
column of the error matrix ~6! with values Eij # 1 at dyl 5 0.1: ~a!
The influence of inaccuracies in the measurement of T, Rf, and Rm
in the determination of n. ~b! The influence of inaccuracies in ns,
nm, and km on the determination of n. The terms of km have
values of #0.1 over the whole n–k plane, and only the contours
with values of 0.1 are plotted.
latter is measured more imprecisely, i.e., DRyR is
higher.
The situation is similar for the accuracy of deter-
mining k, the difference being that the region is ex-
panded to values of k ' 4, especially at n . 2–2.5.
Obviously, the values of the error matrix terms can
provide information about the measured quantities
that are critical to the error in determining n, k, and
d.
2. Assessment of the Maximum Relative Errors
TRR methods make possible the determination of
film thickness. Figure 2 displays the regions in the
n–k plane, defined by the relative errors in d # 4% at
various values of dyl. We see that at dyl ' 0.1
there are large areas in the n–k plane, where d is
determined with a small error. For a short l this
error is much smaller than the error in the measured
Fig. 2. Regions in the n–k plane, defined by the relative error in
d # 4% at various values of dyl.
film thickness when, for example, profilometer Taly-
step with an accuracy of 65 nm is used. Note that
the accurate determination of d makes possible the
reliable isolation of the correct physical solutions for
n and k.
Figures 3~a! and 3~b! show the regions in the n–k
plane defined by the maximum relative error in n and
k # 4% at various values of dyl. Comparing Fig.
1~a! and Fig. 3~a! at dyl 5 0.1, we see that in general
the areas of more accurate determination of n coin-
cide with the areas in which all terms of error matrix
have values Eij # 1.
We see from Figs. 3~a! and 3~b! that for a thin film
with a certain thickness the extraction of n and k in
a wide spectral range will be with different accuracy,
depending on the wavelength, i.e., dyl. Generally,
when the thin-film thickness is varied, n and k can be
determined accurately enough in the whole spectral
range of 400 –1000 nm, if they are in the areas of
small errors, i.e., n . 1.5 and k , 3–4.
We also may conclude from Figs. 3~a! and 3~b! that
the TRRm methods make possible the determination
of both n and k with good accuracy in nearly the same
areas of the n–k plane.
B. Maximum Relative Errors in TR Methods
Figures 3~c!–3~f ! show the areas in the n–k plane
where n and k are determined by ~TRf ! and ~TRm!
methods with a maximum relative error of #4% at
various values of dyl. In this case a relative error of
64% is assumed in thickness d, corresponding to the
relative error in the thickness determination by the
~TRf Rm! method shown in Fig. 2.
Comparing Fig. 3~c! with Fig. 3~e!, we see that the
TRf method yields more accurate solutions for n at
smaller dyl in the region n . 2–2.5 and k , 2–2.5.
By contrast the TRm method has wider areas of more
accurate solutions for k @Figs. 3~d! and 3~f !#.
Unlike in TRRm methods, in TR methods the areas
with more accurate solutions for n and k overlap to a
much lesser extent ~Fig. 3!; i.e., in most cases, if one
of the quantities is evaluated with better accuracy,
the other is determined with greater error.
Comparing the results in Fig. 3 shows that each
method can give good accuracy for n and k, depending
on the optical parameters of the investigated thin
film and the spectral range. Obviously all the meth-
ods should be employed in combination, and the most
accurate solutions for n and k should be selected from
the corresponding areas, as demonstrated below.
C. Maximum Errors in the Method T~k 5 0!
Figure 4 depicts the n–dyl plane with contours des-
ignating the maximum relative errors in the deter-
mination of n. In this case Ddyd 5 64% is assumed,
corresponding to the relative error in d as determi-
nated by the TRf Rm method. The areas with very
high errors are in the vicinity of the curves for which
~]Ty]n! 5 0, i.e., around the transmission curve max-
ima. Obviously at k 5 0 this method is preferable in
a wide range of dyl, provided fairly accurate deter-
mination of d by the TRf Rm method is applied.
1 July 1998 y Vol. 37, No. 19 y APPLIED OPTICS 4263
Fig. 3. Regions in the n–k plane, defined by the relative error in n and k # 4%, at various values of dyl:
and ~e!, ~f !, ~TRm! method.
4. Application of the Error Analysis
Next we illustrate the application of the error anal-
ysis to the method selection and to the most accurate
determination of the thickness and the optical con-
stants of thin films.
A. Sample Preparation and Spectrophotometric
Measurements
The thin films of As2S3 and Sb2Se3 were produced by
vacuum thermal evaporation of the substances11,12 on
planetary moving substrates, which ensures excel-
lent uniformity of the thin film. Pieces of Si wafers,
whose surface was cleaned9 before film evaporation,
were fixed to the preliminary cleaned glass sub-
strates ~BK7! with high surface flatness.
The absolute reflectance and the transmittance of
the samples were measured with a spectrophotome-
ter Cary 5E at normal light incidence in the spectral
range of 400 –1000 nm. The measured values of the
transmittance T and the absolute reflectance Rf, Rb,
Fig. 4. T~k 5 0! method: solid curves, contours of the relative
error in n with the indicated values, plotted in the n–dyl plane;
dashed curves, contours plotted for ~]Ty]n! 5 0, showing the areas
of uncertainty of the method in extracting n.
4264 APPLIED OPTICS y Vol. 37, No. 19 y 1 July 1998
~a!, ~b!, ~TRf Rm!; ~c!, ~d!, ~T Rf !;
and Rm of the samples of As2S3 and Sb2Se3 thin films,
deposited on BK7 and Si substrates, are given in
steps of 50 nm in Table 1.
B. Determination of the Thickness and the Optical
Constants
T, Rf, and Rb of the thin films were evaluated from
the photometric quantities by Eq. ~10!; n, k, and d
were determined by the ~TRf Rm!, ~TRf !, and ~TRm!
methods. Figure 5 displays all solutions for thick-
ness d derived from the TRf Rm method and the ac-
curacy for the correct solutions. As seen, the only
solutions with one and the same film thickness in the
whole spectral range are 58 6 1.6 nm for As2S3 and
78 6 0.9 nm for Sb2Se3. The indicated values and
the maximum errors are taken from the spectral
range, corresponding to the most accurate determi-
nation of d, marked with arrows in Figs. 5~b! and
5~d!.
Obviously, the correct physical solutions for n and
k correspond to these thicknesses, and they are given
in Figs. 6 and 7 with the corresponding absolute er-
rors. In the same figures we also display the values
of n and k evaluated by the ~TRf ! and ~TRm! methods,
using the iteration Newton–Raphson’s method13 and
the corresponding errors calculated at the aforemen-
tioned accuracy of d. Only values corresponding to
the true solutions from the ~TRf Rm! methods were
accepted.
Figure 8 presents the solutions obtained for n by
the T~k 5 0! method for the spectral range in which
k 5 0.
Figures 6 – 8 reveal that the methods used provide
solutions with different accuracy in the spectral
range of 400 –1000 nm. Obviously, for n of the As2S3
film the most accurate solutions are from 400 to
550 nm by the ~TRf Rm! method and from 550 to 1000
 Table 1. Spectrophotometric Quantities T, Rf, Rb, and Rm of As2S3 and Sb2Se3 Samples

As2 S3 Sb2 Se3

l
~nm! T~%! Rf ~%! Rb~%! Rm~%! T~%! Rf ~%! Rb~%! Rm~%!

400 43.5 24.3 19.2 28.8 2.5 30.6 20.4 32.4

450 53.7 35.4 33.5 19.5 5.7 28.7 17.9 32.8
500 58.2 39.9 39.3 9.8 11.5 25.0 14.0 32.6
550 60.9 39.1 38.8 5.0 20.9 21.2 11.1 31.9
600 63.0 37.0 36.8 4.8 32.7 21.9 14.3 30.7
650 65.1 34.9 34.7 6.4 41.9 29.7 25.1 29.5
700 67.1 33.0 32.8 8.5 45.8 39.6 37.4 28.1
750 69.1 31.1 30.9 10.7 46.6 46.9 46.3 25.9
800 70.7 29.1 29.1 12.8 47.0 51.6 51.3 23.4
850 72.3 27.5 27.6 14.5 47.4 53.0 53.2 21.1
900 73.7 25.9 26.0 16.1 47.7 52.8 52.9 19.3
950 74.9 24.5 24.5 17.7 48.0 52.3 52.4 18.2
1000 76.0 23.4 23.4 18.8 48.7 51.1 51.3 17.7

Fig. 5. Solutions for film thickness d by the ~TRf Rm! method and absolute error in d for the correct values @d~l! ' const#: ~a!, ~b!, As2S3
films, d 5 58 6 1.6 nm; and ~c!, ~d!, Sb2Se3 films, d 5 78 6 0.9 nm.

Fig. 6. Dispersion curves of n and k and their absolute errors for As2S3 ~d 5 58 6 1.6 nm!, obtained by the three designated methods.

1 July 1998 y Vol. 37, No. 19 y APPLIED OPTICS 4265

Fig. 7. Dispersion curves of n and k and their absolute errors for Sb2Se3 ~d 5 78 6 0.9 nm!, obtained by the three designated methods.
Fig. 8. Dispersion curves of n and the absolute errors, obtained by
the T~k 5 0! method for As2S3, d 5 58 6 1.6 nm and Sb2Se3, d 5
78 6 0.9 nm.
Fig. 9. Dispersion curves of n and k and the corresponding abso-
lute errors, assembled from the spectral ranges with maximum
accuracy of the used methods for ~a!, As2S3, d 5 58 6 1.6 nm; and
~b! Sb2Se3, d 5 78 6 0.9 nm.
4266 APPLIED OPTICS y Vol. 37, No. 19 y 1 July 1998
nm by the T~k 5 0! method, while for k they are in the
whole spectral range by the ~TRf Rm! method.
For the Sb2Se3 thin films the most accurate solu-
tions for n are from 400 to 760 nm by the ~TRm!
method and from 760 to 1000 nm by the ~TRRm!
method, whereas for k they are from 400 to 700 nm by
the ~TRm! method and from 700 to 1000 nm by the
~TRf Rm! method. Figure 9 displays the n and the k
values and the maximum accuracy in the whole spec-
tral range, assembled from the spectral ranges, spec-
ified above.
5. Conclusions
Based on a complete analysis of the maximum errors
in extracting the optical constants and the thickness
of thin films, using photometric measurements at
normal light incidence in the spectral range of 400 –
1000 nm, we can draw the following major conclu-
sions:
~1! Each method, ~TRf Rm!, ~TRb Rm!, ~TRf !, ~TRm!,
and T~k 5 0!, can give good accuracy of n and k,
depending on the optical parameters of the investi-
gated thin film and the spectral range.
~2! In general, the methods using glass substrates
with ns ' 1.5 and the Si substrate are applicable to
values of n . 1.5, k , 4–5, and dyl 5 ~0.02–0.3! with
an accuracy of better than 64%.
~3! In evaluating the optical constants in a wide
spectral range and isolating the correct physical so-
lutions reliably, the best approach is to apply all
methods, analyze the errors, and use the solutions
with the lowest errors in the corresponding spectral
range, as shown in the examples above.
~4! The coefficients in the error matrix can supply
information about the measured quantities that af-
fect most critically the error in determining n, k, and
d.
~5! The ~TRR! methods have the advantage that
they make possible the very accurate determination
of the film thickness and the reliable isolation of the
correct physical solutions of n and k.
The authors are particularly indebted to V. Panay-
otov, who participated at the start of the present
investigation. We are also grateful to B. Medni-
karov and D. Dimitrov for preparing the As2S3 and
the Sb2Se3 films.
This research was accomplished with the financial
support of the Bulgarian Ministry of Education and
Sciences under contract X-624y96.
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