.

Thin Solid Films 313314 1998 177182

Dielectric function modeling for In Al As on InP
1yy y
Leonard I. Kamlet, Fred L. Terry Jr.
U
Department of Electrical Engineering and Computer Science, 111 DTM Bldg., The Uniersity of Michigan, 2360 Bonisteel Bld.,
Ann Arbor, MI 48109-2108, USA
Abstract
. The pseudo-dielectric functions for In Al As on InP 0.305FyF0.635 were measured using spectroscopic ellipsometry
1yy y
over the 1.55.6 eV photon energy range. The layer compositions were measured using double crystal X-ray diffraction. The
pseudo-dielectric functions were t using a critical point-based approach, and a numerical dielectric function model was
generated with the Al fraction, y, as the only free variable. The extracted optical responses were used in process monitoring
applications. 1998 Elsevier Science S.A.
Keywords: InAlAs dielectric functions; Dielectric function modeling; Process monitoring; Strained layer epitaxy
1. Introduction
The lattice-matched In Al AsrIn Ga AsrInP
1yy y 1yx x
materials system is used in a growing number of high
frequency communication and optoelectronic inte-
grated circuit applications. In some cases, small
amounts of strain are intentionally introduced into
the epitaxial layers to change electrical andror opti-
cal properties. Also, variations in epitaxial growth
systems will produce unintended compositional
.
changes and, therefore, changes in the lm strain .
For In Al As on InP, there is only one composi-
1yy y
.
tion yf0.48 at which the two materials are lattice-
matched. Thin epitaxial lms are under compressive
.
strain for In-rich lms y-0.48 , and under tensile
.
strain for Al-rich lms y)0.48 . The dielectric func-
tions of the epitaxial lms are changed by both com-
w x
position and strain effects 13 .
It has been well established that spectroscopic el-
.
lipsometry SE and normal-incidence spectral reec-
.
tometry SR can be used for highly accurate non-de-
structive lm thickness measurements on multilayer
structures provided that the dielectric functions of the
U
Corresponding author. Tel.: q1 734 7639764; fax: q1 734
9360347; e-mail: fredty@umich.edu
materials in the layers are known. However, use of
inaccurate dielectric function data in reection-based
thickness measurements can lead to signicant thick-
ness errors. Therefore, accurate dielectric functions
.
and a parametric model as a function of y for
In Al As are needed for run-to-run epitaxial
1yy y
growth control, reactive ion etch control, and other
room-temperature process monitoring applications.
The dielectric function of In Al As on InP has
0.52 0.48
been previously reported for the 2801900 nm wave-
. w x
length range ;0.65 to 4.43 eV 4 and the composi-
tion-dependent refractive indices of In Al As on
1yy y
GaAs have been reported at laser wavelengths of
w x
632.8 nm and 1530 nm 5 . However, the dielectric
functions of In Al As on InP in the near infrared
1yy y
to near ultraviolet range have not been widely re-
ported for non-lattice matched compositions. In this
paper, we will present the pseudo-dielectric functions
.
for ve compositions ys0.305, 0.44, 0.48, 0.55, 0.635
of In Al As. We will discuss a composition-depen-
1yy y
dent parameterization for the complex dielectric func-
tion for these pseudo-dielectric functions. We de-
scribe our parameterization scheme, which is an ex-
tension of the critical point parabolic band method of
w x
Kim 6,7 . This is a phenomenological method which
is based on single electron transitions in the semicon-
0040-6090r98r$19.00 1998 Elsevier Science S.A. All rights reserved
. PI I S0 0 4 0 - 6 0 9 0 9 7 0 0 8 0 7 - 9
( ) L.I. Kamlet, F.L. Terry Jr. rThin Solid Films 313314 1998 177182 178
ductor, and has been previously used for composition-
dependent parameterization of the dielectric func-
w x
tions for lattice-matched materials systems 810 . In
this paper, we will present a rst application of this
method to strained layer materials.
.
We will also show results using the InAlAs
data in the analysis of small spot spectral reectome-
.
try data in two process monitoring applications: i
mapping of as-grown epitaxial layer uniformity; and,
.
ii the development of an electron cyclotron reso-
.
nance ECR reactive ion etch process for the base
contact of an InAlAsrInGaAsrInP heterojunction
.
bipolar transistor HBT .
2. Experimental details
.
Five samples were grown on 001 Fe-doped InP
substrates by solid-source molecular beam epitaxy
.
MBE in a Riber 2300. The layers were grown at a
substrate temperature of 490C with an As pressure
of 1.31.4=10
y5
torr. The samples were nominally

;10 A InGaAsrIn Al AsrInP samples with ys

1yy y
0.3050.635. The InGaAs capping layer was grown
under ux conditions that produce lattice matched
material in steady state growth. The capping layer was
incorporated to suppress oxidation of the Al-contain-
ing lm and possible optical complications due to
oxidation-induced roughness. All target thicknesses
were below the Matthews-Blakeslee critical thickness
w x
11 for the given composition; however, in some cases
this thickness was exceeded, creating the possibility of
incoherent strain in those lms.
Compositions were determined using double crystal
.
X-ray diffraction DCXRD . Rocking curves from the
.
004 reection were obtained using a Rigaku diffrac-
tometer using the Cu K wavelength. The lm com-

position was determined using a program based on

w x
dynamical X-ray scattering theory 12 and Vegards
law.
Spectroscopic ellipsometry data were collected us-
ing a Sopra GESP-5 system over the 1.55.6 eV range
in increments of 0.01 eV. The instrument was oper-
ated in the tracking analyzer mode. We used two
separate prism-grating monochromators, one of which
was optimized for UV operation. Data were collected
on both monochromators between 2 and 3 eV and
examined to ensure consistency of the two data sets.
The monochromator change-over was done during
the collection of data from each sample to avoid
variations in sample alignment. Data that did not
.
agree to be better than 0.01 in both tan and
.
cos were recollected following realignment of the
sample. SE data were collected at both 70 and 75
angles of incidence. We intended to collect data below
the fundamental band edge, but the combined effects
of reection from the back surface of the sample, the
.
well-known difculties of measuring at low tan
conditions with rotating-polarizer ellipsometers, and
the increased noise of the InGaAs near-infrared de-
.
tector vs. the UV-visible photomultiplier made these
data unreliable.
3. Results and discussion
Extraction of the pseudo-dielectric function from
the ellipsometry data was performed using a two-step
process. A complex harmonic oscillator approxima-
. w x
tion CHOA 13 with ve oscillators was used as a
rst model for the InAlAs dielectric response. The
thickness of the InAlAs layer, the InGaAs cap layer
.
plus thin native oxide over-layer , and a CHOA esti-
mate of the InAlAs dielectric response were de-
termined by non-linear least squares regression using
the Levenberg-Marquardt method. For initial guesses,
.
the 20 parameters four per oscillator for the CHOA
model were found for each composition by using the
values from the next nearest composition and adjust-
ing oscillator energies due to peak shifts. The rst
regression analyses were performed on data for the
.
lattice matched sample no. 1295 with initial guesses
for the oscillator parameters being chosen by assign-
ing oscillators to the E , E q , and E transitions,
1 1 1 2
a broad linewidth oscillator to the region between

E q and E to ll-in the response between the

1 1 2
.
critical points , and a broad linewidth oscillator above
.
E to adjust the baseline and the response .
2
The oscillators associated with the critical points can
be initially estimated by tting to second derivative
data; however, in this case the initial guesses were
chosen by shifting the energies of the corresponding
w x
oscillators from our t to GaAs 13 . The pseudo-
dielectric function for each InAlAs composition was
then extracted on a point by point basis using the
thicknesses found previously from the CHOA t. To
reduce numerical artifacts, we then re-t the CHOA
parameters to the resulting dielectric function and
repeated the two-step process. The data were then

visually examined for interference oscillations thick-

.
ness error-induced effects . Initial guesses for the
regression were adjusted until an apparent best t
was found.
Compositional data were collected by DCXRD as-
suming coherently strained lms. In principle, the
Pendellosung fringes of the rocking curves will pro-
vide an independent estimate for the epitaxial lm.
.
However, only the lattice-matched sample no. 1295
.
and one strained sample no. 1296 showed clear
Pendellosung oscillations. This could have been the
result of interface quality problems, but may also be
the result of thickness non-uniformity in the epitaxial
layers. For the strained sample, the extracted thick-
ness from DCXRD was ;29.0 nm based on a t-
( ) L.I. Kamlet, F.L. Terry Jr. rThin Solid Films 313314 1998 177182 179
by-eye alignment of the oscillation peaks and valleys.
The regression procedure described above yielded
27.6 nm from the SE data.
The thickness and composition data are summa-
rized in Table 1. As can be seen, the measured
thicknesses were greater than the growth targets in all
cases, while the measured compositions are very close
to the target values. The reasons for this discrepancy
are not known. However, because of the thicker-
than-desired InAlAs layers, the assumption of coher-
ent strain may be erroneous, and, therefore, our de-
rived model should only be regarded as a rst attempt
at characterizing this material system. A study of both

thinner lms which are more likely to be coherently

.
strained and of thick, fully-relaxed lms at various
Al-fractions is needed. This was, unfortunately, bey-
ond the nancial scope of our project.
To examine further the possibility of relaxation of
the strain, we examined three samples for variations
.
in cos with azimuthal angle at the HeNe laser
.
wavelength 632.8 nm on a Gaertner L116B rotating
analyzer ellipsometer equipped with a rotational stage.
Without surface roughness due to incoherent growth,
w x
no variation with azimuthal angle is expected 14 .
The results are shown in Fig. 1. The lattice matched
.
sample no. 1295 was analyzed, and the results can
be regarded as an error bound for this measurement,
as there should be no variation for this sample. These

variations introduce signicant uncertainties as large

.
as 53% for sample no. 1298 in the values of the
imaginary part of the dielectric function, , but
2
.
relatively small errors ;1% or less for the real part,
. Furthermore, at this wavelength is small and is
1 2
therefore subject to large errors in extraction from
rotating element ellipsometry. We have not yet syste-
matically studied the azimuthal anisotropy of these
samples at other wavelengths, but a few SE measure-
ments taken at different substrate orientations did
not indicate large differences at the shorter wave-
lengths. Another possible cause of the observed azi-
muthal variations is that in some cases the InAlAs

thicknesses are non-uniform across the samples as

.
will be shown later , leading to possible sensitivity in
the precise beam location during measurement. Other
well-documented ellipsometry alignment issues, such
as beam wobble, may also be a factor due to the layer
thickness non-uniformity.
The extracted pseudo-dielectric functions of the
samples were tted using the modications to the
Kim-Garland approach which we have presented pre-
viously for the dielectric functions of lattice-matched
w x
In Ga As P on InP 10 . This parameterization
1yx x y 1yy
scheme assumes that the dielectric function is
isotropic and that the semiconductor is unstrained.
The optical anisotropy expected in uniaxial III-V
compounds is difcult to resolve with ellipsometry, as
the angle of refraction varies only slightly with angle
of incidence due to the high refractive index. Aspnes
has examined this problem and notes that for rela-
< < .
tively high dielectric constant materials ;10 the
surface normal component of the dielectric function
will have little effect on the ellipsometrically mea-
sured pseudo-dielectric function and that the mea-
sured pseudo-dielectric function is the projection of
the dielectric function tensor onto the line formed by
the sample surface and the measurement plane of
w x
incidence 15 . De Smet has shown numerically that
even for the case of uniaxial crystals, multiple angle
of incidence ellipsometry measurements are insuf-
cient to measure the normal and extraordinary com-
w x
ponents of the dielectric function separately 16 .
Therefore, we ignore optical anisotropy in our model.
In principle, the dielectric function model should
be modied to account for changes in the band struc-
ture due to strain. The most signicant effects are
shifts in the energies, amplitudes, and linewidths of
w x
the critical points 13,17 ; however, these effects
must be treated in any composition-dependent
parameterization problem. The parameters needed to
estimate the energy, amplitude, and linewidth changes
accurately as a function of composition would pre-
sumably be different for the strained vs. the relaxed
case, but no other changes in the parameterization
scheme should be needed due to these effects. We
expected that the most signicant effects which would
require changes in the model formulae to be the
reduction in degeneracy and reduction of dimension-
. . w x
ality of the E X and E K transitions 18 . We
2 2
modied the Kim-Garland expression to include a
two-dimensional critical point for parallel strain and a
Table 1
A summary of the targetes thickness and compositions of the InAlAs samples studied, and the thicknesses and compositions obtained by SE
and DCXRD
Sample no. Target thickness Target Al SE thickness DCXRD Al Critical thickness
. . . nm fraction nm fraction nm
1295 300.0 0.48 430.4 0.480
1296 15.0 0.33 27.6 0.305 23.25
1297 70.0 0.43 119.6 0.440 93.56
1298 70.0 0.53 102.7 0.550 76.81
1299 15.0 0.63 33.4 0.635 21.21
( ) L.I. Kamlet, F.L. Terry Jr. rThin Solid Films 313314 1998 177182 180
. Fig. 1. Variation in cos at s623.8 nm with azimuthal angle
. for the latticed matched lm no. 1295 and two strained layer lms.
one-dimensional critical point for perpendicular
.
strain. For a uniaxial crystal grown in the 001 direc-
tion, both types should occur.
We t the dielectric functions using the methods
w x
detailed in earlier work 610,18 . The quality of the
extracted pseudo-dielectric functions was not suf-
cient to support second and third derivative tting
methods. Therefore, only the pseudo-dielectric func-
tions and their rst derivatives were used in the ts.
Very good ts to the primary data were achieved, but
the lack of higher derivative data increases the con-
dence limits that can be placed on the critical point
energies and lineshapes. In all cases the use of the
reduced-degeneracy formulation resulted in worse ts
than the isotropic formulation; therefore, only the
isotropic results will be shown. The reasons for this
are not clear, but possibilities include incoherent
strain effects or insufcient resolution in our experi-
mental data.
Two separate ts using the modied Kim parame-
terization scheme were performed. First, the model
parameters were optimized for each composition in-
.
dependently individual ts . Second, a composition-
dependent parametric model was generated by a
global optimization over all the data sets. The individ-
ual data and ts are shown in Fig. 2a and b. The E
1

and E q critical point energies along with

1 1
.
parabolic ts of the energies vs. y from the individual
ts are shown in Fig. 3. The variation of these ener-
gies follows the trend expected from the critical point
energies of the relaxed binary endpoints of InAs and
AlAs. Also, the amplitude of the E critical point
1
increased relative to that of the E q critical point
1 1
as the In concentration was increased, and the oppo-
site occurred as the Al concentration was increased.
Unfortunately, no strong conclusions can be drawn
regarding the strain state of the epitaxial lms from
these observations, as both are consistent with what
Fig. 2. The measured and best t pseudo-dielectric functions for
. . the InAlAs lms studied here; a real part, b imaginary part.
would be expected from compositional changes as
w x
well as strain-induced changes 1,3 . The strong
strain-induced reduction of the E q energy shift
1 1
vs. In content for strained layers of InGaAs on GaAs
w x
observed by Pickering 19 is not evident in this data.
This may also be an indication that our lms are not
coherently strained. Only a small shift in the E
2
critical point was observed.
The composition-dependent model was generated
using the following procedure. The energies from the
individual ts were tted to quadratic polynomial
functions of the Al fraction y, and the linewidths to
cubics using the DCXRD-determined y values. These
factors were then held constant and the amplitude
factors were tted as cubic functions of y by simulta-
neously considering all data sets. Nearly equivalent
quality ts to the measured data were obtained in all
( ) L.I. Kamlet, F.L. Terry Jr. rThin Solid Films 313314 1998 177182 181
. . Fig. 3. The E round points and E q square points critical
1 1 1
point energies from our parameter optimization for individual ts
vs. the Al fraction, y. The dashed lines are quadratic functions
tted to these critical point energies.
. w x
cases visually equivalent to the plots of Fig. 2 20 .
.
For example, the root mean square error MSE ,
2 2
meas f i t meas f i t
. .
y q y rN where N '
/ E 1 1 2 2
is the number of points, and the summation is over
.
the measured photon energies, E , for the individual
.
t to the lattice matched data no. 1295 was 0.217
while that of the composition-dependent t was 0.361.
The error per point is typically well below 1% for

both and except for a narrow error spike

1 2
.
;"10% around E . As all available data were
2
needed for the compositional t, an objective test of
the accuracy in extracting y for an intermediate com-
position could not be run.
We have made use of the InAlAs pseudo-dielectric
function data in two process monitoring applications.
The extracted pseudo-dielectric function data from
sample no. 1297 were used in a Leitz MPV-SP micros-
.
cope-based spectral reectometer SR with an auto-
mated stage to map the thickness uniformity of the
growth run. The sample was not rotating during
growth, and the growth conditions were not optimized
for uniformity at this composition. The resulting non-
uniformity is evident in the thickness map of Fig. 4. A
sample from the thicker left edge of this wafer was
measured by XTEM, and yielded about ;150 nm
.
lm thickness sample preparation was not optimal in
at least qualitative agreement with the SR map. In a
second application, we have used these data for pre-
and post-ECR etch thickness measurements of In-
AlAsrInGaAsrInP HBT device structures. The start-
ing InAlAs and InGaAs could be determined and
mapped for uniformity on the SR. These thicknesses
were used in estimating required etch times. As an
example, one pre-etch measurement yielded thick-
nesses of 186"1 nm of InAlAs on top of 63.5"0.5
nm of InGaAs from the data shown in Fig. 5. Use of
Fig. 4. A wafer map obtained by automated microscope-based spectral reectometry of the InAlAs thickness on sample no. 1297.
( ) L.I. Kamlet, F.L. Terry Jr. rThin Solid Films 313314 1998 177182 182
. Fig. 5. The reectance vs. wavelength data points and best t
. solid curve for an InAlAsrInGaAsrInP HBT test structure yield-
ing 186"1 nm of InAlAs over 63.5"0.5 nm of InGaAs.
this procedure in verifying the accuracy of an optical
emission endpoint detection scheme will be described

in a separate publication Hanish et al., unpublished

.
results .
4. Summary
We have made an initial investigation of the dielec-
tric functions of In Al As epitaxial lms grown on
1yy y
InP and have parameterized the ts to produce a
numerically efcient compositional model for use in
process monitoring applications. Our original intent
was to examine coherently strained lms so that the
paramaterization results could be applied to moni-
toring applications in which variations around the
nominally lattice-matched case are encountered.
However, as discussed above, the lms in our study
may not be coherently strained. Additional studies of
coherently strained and fully relaxed lms in this
materials system are needed.
Acknowledgements
This work was supported in part by DARPA under
contract F33615-92-C-5972. The authors would also
like to thank Drs. Xiangkun Zhang and Pallab K.
Bhattacharya for growth of the MBE samples, and
Arun Ramamoorthy for performing the TEM analy-
sis. We would also like to thank the State of Michigan
Center for Display Technology and Manufacturing for
use of the GESP-5.
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