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Thin Solid Films 313]314 Ž1998.

620]624

Ellipsometric and reflectance-anisotropy measurements


on rotating samples

K. Haberland a,U , O. Hunderi b , M. Pristovsek a , J.-T. Zettler a , W. Richter a


a
¨ Berlin, Institut fur
Technische Uni¨ersitat ¨ Festkorperphysik,
¨ Sekr. PN 6-1, Hardenbergstr. 36, D-10623 Berlin, Germany
b
Uni¨ersity of Trondheim, Norwegian Institute of Technology, Dept. of Physics, N-7034 Trondheim, Norway

Abstract

Device grade semiconductor epitaxial growth is usually performed on rotating substrates in order to achieve uniform layer
thickness and composition. This often complicates in-situ optical measurements for growth control. Therefore, in this paper
we present a method that significantly reduces the signal distortions imposed on RAS Žreflectance anisotropy spectroscopy.
and ellipsometry spectra by rotating and wobbling samples. Several cases Žphase and frequency of the sample rotation either
known or unknown, wobbling and ideally rotating samples. are investigated and the respective optimized experimental set-ups
are presented for both RAS and ellipsometry. Q 1998 Elsevier Science S.A.

Keywords: Ellipsometry; Reflectance anisotropy spectroscopy; Real-time monitoring; In-situ spectroscopy

1. Introduction even the slightest changes to the well-running growth


system. Therefore, in this paper we present an optical
In most production-line epitaxial growth systems set-up that would leave the growth system completely
sample rotation during layer deposition is essential unchanged because it is based on a passive compensa-
for obtaining the required thickness and composition tion of the light beam deviations caused by the
homogeneity across the wafer. On the other hand wobbling sample. All experiments have been per-
sample rotation and sample wobbling significantly formed, however, ex-situ on an optical bench with
complicate in-situ optical measurements such as spec- sample wobbling added intentionally for optimizing
troscopic ellipsometry ŽSE. and reflectance-aniso- and testing the suggested set-up. An ordered InGaP
tropyrdifference-spectroscopy ŽRASrRDS.. Ž001. sample was used because it gives a large RAS
Several approaches dealing with rotating and signal even in air and at room temperature w2x.
wobbling samples in SE and RAS have recently been
published Žw1x; Ebert et al., unpublished results .. In 2. RAS on rotating samples
general the idea of these approaches is to reduce the
magnitude of wafer wobbling to a minimum by intro- In Fig. 1 the modified set-up is shown for RAS
ducing additional mechanical andror electronic sys- measurements on rotating and wobbling samples. The
tems compensating the unwanted deviations of the passive compensation of the effects of sample
sample from the optimum position for in-situ mea- wobbling is achieved by the additional implementa-
surements. However, it is not favored to implement tion of a spherical mirror ŽSM. w3x and a beam-splitter
ŽBS. into the standard RAS system of Aspnes et al.
w4x. With the sample positioned exactly at the center
U of curvature of the spherical mirror, every ray re-
Corresponding author. Fax: q49 30 31421769; e-mail:
habi@gift.physik.tu-berlin.de flected by the sample is reflected back to itself by the

0040-6090r98r$19.00 Q 1998 Elsevier Science S.A. All rights reserved


PII S0040-6090Ž97.00897-3
K. Haberland et al. r Thin Solid Films 313]314 (1998) 620]624 621

Fig. 1. Schematic set-up for RAS. L, XBO-lamp; P, polarizer; BS, beam splitter; S, rotating sample; SM, additional spherical mirror; PEM,
photoelastic modulator; A, analyzer; MC, monochromator; D, detector. Note that the sample is placed at the center of curvature of the mirror
SM.

spherical mirror and then returns to the beam splitter actual azimuth of the sample is known while per-
via the second reflection from the sample. After pass- forming the in-situ optical measurements. Under these
ing the beam-splitter the state of polarization of the conditions the RA of the sample can be calculated
light is analyzed as usual by the PEM-polarizer-detec- from every single measurement except for only a few
tor system. The double reflection on the sample re- azimuths where the anisotropy just cancels out w5x.
sults in the additional advantage of the anisotropy The spectra in Fig. 3 have been taken under such
signal having twice the amplitude compared to a experimental conditions. The measured anisotropy
conventional RAS measurement. Since one needs to signal D rrr is given by:
avoid the beam being reflected directly back into the
slit of the spherical mirror at any moment, the angle Dr r w110x y r w110x
s h cos Ž 2 a . 2 Ž1.
of incidence w is set to ; 58 Ž w ) 2D w .. r r w110x q r w110x
The degree of passive wobble compensation that
can be reached by this method is surprisingly high with a being the sample’s azimuth and h an elec-
Žsample deviations D w of nearly two degrees from the tronic damping parameter. The electronic damping
mean position are acceptable. and depends mainly on constant h is due to the time constant of the RAS
the proper adjustment of the additional spherical electronic detection system and has been determined
mirror. Fig. 2 shows RAS transients for both well-ad- by reference measurements on non-rotating samples.
justed and badly-adjusted mirrors taken on a sample
rotating at 0.2 Hz that was intentionally misaligned by
several degrees. This wobble amplitude would be far
too high for RAS data collection with a conventional
set-up. The reflected beam simply would not pass
through the PEM aperture. In both transients the
2 v-signal carrying the polarization information can
be seen. In the upper transient, however, due to the
badly aligned SM, there is also the 1 v-component
present caused by the sample wobbling.

2.1. RAS measurements with the actual sample azimuth


known (synchronized measurements)

Fig. 2. RAS transients at 3.47 eV for SiŽ110.. ŽA. Badly adjusted


In some growth systems Že.g. MBE chambers with auxiliary spherical mirror, ŽB. properly adjusted spherical mirror
sample-rotation stages driven by stepper motors. the Ž n s 0.25 Hz, 2D w s 1.58..
622 K. Haberland et al. r Thin Solid Films 313]314 (1998) 620]624

In Fig. 3 RAS spectra taken on a rotating and wobbling


InGaP sample are given. The RA signal detection was
synchronized by the trigger pulses driving the stepper
motor that rotates the sample. Obviously, due to the
passive optical compensation of the sample wobble,
both the real and imaginary parts of the anisotropy
signal can be measured directly and in real-time.
Generally, even fluctuations of the rotation frequency
are acceptable for performing precise RAS measure-
ments when the data on the rotating and wobbling
sample can be collected synchronously, i.e. triggered
by the sample stage, and when the time constant of
the RAS electronics is set to sufficiently small values.

2.2. RAS measurements with the actual sample azimuth


unknown
Fig. 3. RAS spectra of InGaP obtained in the synchronized mea-
There are growth systems in which no reference surement mode Ž n s 1.2 Hz, h s 0.743, 2D w s 1.28..
signal is available giving the actual sample azimuth.
Horizontal MOVPE reactors where the substrate is Again the sample was intentionally misaligned on
placed on a susceptor that rotates in a flow of carrier the rotating sample holder Žrotation frequency v s
gas may serve as an example. Fig. 4 illustrates that 2pn . and the RAS measurements were taken blindly,
precise RAS measurements can be taken even under i.e. without transferring any information regarding the
these rather demanding conditions for in-situ spec- sample azimuth to the RAS system. The measured
troscopy. anisotropy signal is given by Ž1. with a s v t. To deal

Fig. 4. RAS spectra of a rotating and wobbling InGaP sample extracted from the raw data by an FFT-filter algorithm. Ža. The signal measured
directly. Žb. Fourier spectrum of the absolute value of the raw signal. The side bands are caused by the rotation and the central part
represents the RAS signal. Žc. Inverse transformed signal after filtering. Žd. Normalized, corrected and smoothed RAS spectra compared with
corrected spectra Ždashed line. taken on a non-rotating sample Ž n s 0.125 Hz, h s 0.956, 2D w s 1.28, no. of measurement points: 501,
acquisition time per point: 30 ms..
K. Haberland et al. r Thin Solid Films 313]314 (1998) 620]624 623

with this situation, the RAS spectrum was taken with spherical mirror used. The maximum rotation fre-
a large number of energy set-points and with a fixed quency depends only on the time resolution of the
delay time between these points. The spectrum in Fig. RAS system. Assuming a realistic time constant of 10
4a is therefore due to the sample rotation, modulated ms, rotation frequencies up to 10 Hz should be possi-
in amplitude. The carrier frequency is twice the rota- ble Žbased on the Nyquist criterion..
tion frequency v and the modulation amplitude rep- To take advantage of this method, even moderate
resents the RAS signal. To obtain a RAS spectrum variations of the rotation frequency of the sample can
from the raw data shown in Fig. 4a, filtering in Fourier be dealt with by properly adjusting the Fourier filter.
space must be applied. For demodulation, the abso-
lute value of the raw-signal is taken, transformed into 3. Ellipsometry on rotating samples
Fourier space and subsequently filtered by means of a
Gaussian filter of appropriate width. Fig. 4b shows the Fig. 5 shows the set-up used for ellipsometric mea-
Fourier spectrum and the filter. Note that the side surements on rotating samples. Similar to the RAS
bands representing the rotation-induced carrier fre- set-up, the ellipsometer consists of a beam splitter BS
quency are separated from the central part of the and a spherical mirror SM. Due to the double reflec-
Fourier spectrum which represents the RAS informa- tion on the sample in this set-up, instead of the
tion. After applying the filter, the side bands are complex reflectance ratio r s r prr s now
completely eliminated. By this procedure only the
absolute value of the RAS spectrum is achieved ŽFig. r 2 s < r < 2 ? e 2 i ar g Ž r . s tan 2 C ? e 2 iD
4c.. To obtain the complete spectrum the phase-shifts
in the oscillations in Fig. 4a must be analyzed. Then is measured. In contrast to the respective RAS mea-
the sign of the RAS signal is known and can be surements the wobbling of the sample causes an addi-
corrected. This has been done in Fig. 4d where the tional difficulty: variations in the angle of incidence.
measured and corrected RAS spectra are compared The measured ellipsometric parameter < r < is highly
to a reference spectrum measured on a non-rotating sensitive to these changes of the angle of incidence.
sample. Therefore one must either integrate over a suffi-
The spectrum taken by this procedure is automati- ciently large number of rotations or measure additio-
cally corrected for effects caused by residual strain in nally the actual angle of incidence, e.g. by placing a
the windows and by polarization effects due to the four-detector array behind the SM which must be
beam splitter. Again, both real and imaginary parts of partially transparent for a small part of the light.
the RAS spectrum could be measured. Fig. 6 shows ellipsometry spectra of a rotating and
The magnitude of wobbling that can be compen- wobbling Si sample. In the inset a transient at 2.5 eV
sated is only limited by the diameter of the auxiliary is given. Note that cosŽ D . is not affected by the

Fig. 5. Set-up for ellipsometry on rotating samples: L, XBO-lamp; P, polarizer; BS, beam splitter; S, rotating and wobbling sample; SM,
additional spherical mirror; A, analyzer; MC, monochromator; D, detector.
624 K. Haberland et al. r Thin Solid Films 313]314 (1998) 620]624

Fig. 6. Ellipsometric measurements on a rotating Si sample. The short dashed curve is a reference spectrum modeled with w s 668 and 1.5 nm
oxide.

wobbling, while < r < shows oscillations at twice the wobbling samples without implementing any modifi-
rotation frequency. In this case the rotation frequency cation to the sample holder. The set-up presented
was rather high compared to the measurement rate. here facilitates the application of RAS in conventio-
Therefore, by integrating over a large number of nal growth systems and doubles the magnitude of the
rotations, the effect of a changing angle of incidence RAS signal. In SE the passive compensation of sam-
is completely removed from the < r < spectrum. ple wobble significantly complicates the analysis of
For obtaining precise SE spectra, the effect of the ellipsometric measurements because of variations of
beam splitter must be removed from the spectra. the angle of incidence. In addition one must cope
Furthermore, for in-situ applications it is important to with low light intensities caused by two reflections
note that in this configuration the windows are passed near the Brewster angle.
twice by the light if the spherical mirror is positioned
outside the growth chamber. Therefore effects due to
the modification of the polarization state of light by Acknowledgements
additional optical components are more serious in
this configuration than in a conventional set-up. The
spectra shown in Fig. 6 are corrected according to The authors are grateful to Kerstin Knorr ŽTU
Berlin. for supplying the InGaP sample and Ingo
y1
< r < s Ž < r < tBS ? < r < rBS . ? ²< r <: Rieck ŽTU Berlin. for valuable discussions regarding
the effects of electronic damping on the RAS spectra.
arg Ž r . s ²arg Ž r .: y Ž DtBS q DrBS . Ž2. The authors also gratefully acknowledge the support
by the BMBF Ž01 BT 310r835. and the DFG
Here the ellipsometric parameter r BS
r,t
describes the ŽSonderforschungsbereich 296..
additional polarization effects caused by the beam
splitter in reflection and transmission. Additionally,
one must deal with low light intensities, because the References
light is reflected twice by the sample at an angle of
incidence near the Brewster angle. Consequently,
while in principle the passive wobble compensation w1x G.N. Maracas, C.H. Kuo, S. Anand, R. Droopad, G.R.L.
works for ellipsometry as well, the practical applica- Sohie, T. Levola, J. Vac. Sci. Technol. A 13 Ž1995. 727.
tion may be restricted to the normal incidence RAS w2x J.S. Luo, J.F. Geisz, J.M. Olson, M.C. Wu, J. Cryst. Growth
measurements discussed in Sec. 2. Žin press..
w3x O. Hunderi, J.-T. Zettler, K. Haberland, Patent No. DE 197
21 044.9, 1997.
4. Summary w4x D.E. Aspnes, J.P. Harbison, A.A. Studna, L.T. Florez, M.K.
Kelly, J. Vac. Sci. Technol. 6 Ž1988. 1327.
We have demonstrated that it is possible to obtain w5x K. Hingerl, D.E. Aspnes, I. Kamiya, L.T. Florez, Appl. Phys.
RAS and ellipsometric spectra on rotating and Lett. 63 Ž1993. 885.

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