Applied Surface Science 252 (2006) 7275–7278

www.elsevier.com/locate/apsusc

SIMS analysis of a multiple quantum well structure in a

vertical cavity surface emitting laser using the
mixing-roughness-information depth model
S. Ootomo *, H. Maruya, S. Seo, F. Iwase
Yokohama R&D Laboratories, The Furukawa Electric Co. Ltd., 2-4-3 Okano, Nishi-ku, Yokohama 220-0073, Japan
Received 12 September 2005; accepted 15 February 2006
Available online 9 May 2006

Abstract
We have analyzed a multiple quantum well (MQW) structure in a vertical cavity surface emitting laser (VCSEL) epitaxial wafer using
secondary ion mass spectrometry (SIMS). The two energy sputtering method is a very powerful method for providing a depth profile of a GaAs/
Al0.2Ga0.8As MQW with a sufficient depth resolution and a large number of data points in a practical measurement time. This method consists of
rapid high-energy sputtering for a top mirror layer and subsequent low-energy sputtering for an active layer. The resulting profiles were
quantitatively evaluated using the mixing-roughness-information depth (MRI) model. The values of C concentration in modulation-doped
Al0.2Ga0.8As barrier layers have been extracted from the original in-depth concentration profile reconstructed by the MRI model. The relationship
between depth resolution of the resulting profile and surface morphology measured by atomic force microscopy (AFM) is also discussed.
# 2006 Elsevier B.V. All rights reserved.

Keywords: SIMS; VCSEL; MRI model; AFM; Surface roughening

1. Introduction procedure is required. The mixing-roughness-information depth

A vertical cavity surface emitting laser (VCSEL) has become
an optoelectric device with promising applications in optical
computing and optical interconnect applications [1]. Secondary
ion mass spectrometry (SIMS) has been widely used for
measuring dopant profiles in semiconductor materials. Opto-
electric devices containing a multiple quantum well (MQW)
structure in an active region demand high depth resolution to
resolve the individual barrier and well layers. Lower energy
sputtering, often used to obtain a depth profile with a higher depth
resolution of the order of nanometers, may seem an effective
method. The use of low-energy primary ions, however, causes
extremely long measurement time, since deep sputtering of a top
distributed Bragg reflector (DBR) mirror with several micro-
meters in thickness on an active region is performed.
The two energy sputtering method has been reported useful to
obtain a high depth resolution in a deep region [2]. In order to
extract original in-depth distribution from a measured depth
profile, moreover, either convolution procedure or deconvolution
(MRI) model developed by Hofmann [3,4] is a trial and error
approach optimizing the fit of the convoluted profile to the
measured one using three parameters: atomic mixing, w; surface
roughness, s and information depth, l. If it is assumed that the
matrix effects (i.e. change of ionization probability and sputtering
rate in different materials, etc.) are small enough, the original in-
depth distribution of elements can be produced by the MRI model.
In this paper, we have described the two energy sputtering
method to obtain a high resolution depth profile of an MQW
structure in a VCSEL wafer in a practical measurement time.
This method is based on rapid sputtering of a top DBR mirror
by high-energy primary ions and subsequent measurement of
an MQW structure by low-energy primary ions. The resulting
profile has been quantitatively evaluated using the MRI model.
The relationship between roughness parameter, s, involved in
the MRI model and surface morphology measured by atomic
force microscopy (AFM) is also discussed.
2. Experimental details

* Corresponding author. Tel.: +81 45 311 1212; fax: +81 45 314 5190. The sample used in this study is the starting epitaxial wafer
E-mail address: ootomo.shinya@furukawa.co.jp (S. Ootomo). from which 850 nm VCSELs are fabricated. The 850 nm
0169-4332/$ – see front matter # 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.apsusc.2006.02.261
7276 S. Ootomo et al. / Applied Surface Science 252 (2006) 7275–7278

VCSEL wafers were grown by metalorganic chemical vapor

deposition (MOCVD) on GaAs substrates. Their VCSEL
structures consist of an active region embedded between two
DBR mirror layers. The DBR mirrors were composed of a 35-
period Al0.2Ga0.8As/Al0.9Ga0.1As bottom DBR and a 25-period
Al0.2Ga0.8As/Al0.9Ga0.1As top DBR with quarterwavelength-
thick layers. The active region consists of four undoped 6-nm-
thick GaAs quantum wells and five C-doped 10-nm-thick
Al0.2Ga0.8As barriers, centered in Al0.3Ga0.7As cladding layers
to form a l-cavity. For comparison, the VCSEL wafer without a
top DBR mirror layer was also prepared.
The SIMS measurements were performed with quadrupole
PHI-6650 and ADEPT1010 instruments (ULVAC-PHI Inc.).
Negatively charged secondary ions such as AsC
, AlAs
, GaAs

and As
were collected using Cs+ primary ions at the incident
angle of 608. Fig. 1 illustrates the procedure of the two energy
sputtering method to obtain a depth profile of the MQW structure
with a higher depth resolution in a practical measurement time. Fig. 2. SIMS measured, MRI convoluted and reconstructed Al profiles for the
undoped GaAs/Al0.2Ga0.8As MQW structure in the VCSEL sample without the
This method consists of the following two steps. First, the top top DBR layer. The measured depth profiles were obtained by sputtering with
DBR layer is rapidly sputtered using Cs+ beam ions of 10 keV, 1.5 keV Cs+ ions. The obtained parameters are w ¼ 2:0 nm, s = 1.0 nm and
rastered across an area of 500 mm  1000 mm. An average l = 0.4 nm.
sputtering time of one period in the top DBR is 70 s under this
condition. After the complete removal of the top DBR layer, the depth concentration profiles for the MQW structure. The
active region is carefully sputtered with 1.5 keV Cs+ primary ions conversion of the measured AlAs
intensity to Al mole fraction,
scanning over an area of 300 mm  600 mm. The sputtering time x, for the MQW structure was performed using reference thicker
for MQW measurement is approximately 2000 s. The total AlxGa1
xAs (200 nm)/GaAs samples with Al mole fraction
measurement time is approximately 90 min. determined by X-ray diffraction. The AlAs
intensity showed
The AFM measurements of the crater bottoms after the
complete removal of the top DBR layer were performed on a
Nanoscope III system (Digital Instruments) with a scan size of
4 mm  4 mm in air. To avoid the formation of large ripples
with aluminium hydroxide formed on an AlxGa1
xAs surface in
air [5], the sample which had a 25-period Al0.2Ga0.8As/
Al0.9Ga0.1As DBR mirror structure only grown on a GaAs
substrate was prepared for the AFM measurement.

3. Computational details

The calculation based on the MRI model has been used to

reconstruct original in-depth distribution profiles. In this work,
we focused on the reconstruction of the original Al and C in-

Fig. 1. Schematic illustration of the two energy sputtering method for the Fig. 3. (a) Al depth profile and (b) C concentration profile by sputtering with
measurement of the MQW structure in a VCSEL epitaxial layer: (a) high- 1.5 keV Cs+ ions for the modulation-doped GaAs/Al0.2Ga0.8As MQW structure
energy sputtering to remove the DBR mirror rapidly and (b) low-energy after removing the top DBR layer. The obtained parameters are w ¼ 2:0 nm,
sputtering to measure the MQW structure. s = 3.7 nm and l = 0.4 nm.
 S. Ootomo et al. / Applied Surface Science 252 (2006) 7275–7278
Fig. 4. The 4 mm  4 mm AFM images of the crater surface after (a) the 10-keV-sputtering and (b) the subsequent 1.5-keV-sputtering. The rms roughness values of
these images are (a) 2.76 nm and (b) 1.79 nm. The data scale of maximum value is set to 20 nm for both images.
good linearity with Al mole fraction in the range of x = 0–0.4, and
the anomalous change of interface shape at AlxGa1
xAs/GaAs
interfaces is small enough in the range of x = 0–0.3. The
difference of sputtering rate between GaAs and Al0.3Ga0.7As was
within 5%. Therefore, we assumed that matrix effects are
negligible with Al mole fraction in the range of x = 0–0.3.
Kawashima et. al. [6] reported the similar result with their
quadrupole PHI-6650 instrument. On the other hand, the
conversion of the measured AsC
intensity to the C concentra-
tion for the Al0.2Ga0.8As barrier layers was determined using the
C-implanted Al0.2Ga0.8As standard sample. During the proce-
dure of fitting the convoluted profiles to the measured ones, the
atomic mixing w and the roughness parameter s were varied. The
information depth, l, was kept constant during fitting. The l
value of 0.4 nm was used in this study [4].
4. Results and discussion
In order to inspect the influence of deep sputtering of a top
DBR on a depth resolution of an MQW depth profile, the active
layers in the VCSEL without the top DBR were sputtered using a
1.5 keV Cs+ primary ions scanning over an area of
300 mm  600 mm. Fig. 2 shows the measured Al profile of
the GaAs/Al0.2Ga0.8As MQW structure. The convoluted and
reconstructed profiles for Al obtained by the MRI calculation are
also shown in Fig. 2. We can clearly distinguish between
individual GaAs well and Al0.2Ga0.8As barrier layers. The fitting
parameters used for the Al depth profile were w ¼ 2:0 nm,
s = 1.0 nm and l = 0.4 nm. However, the sputtering rate of
0.09 nm/s is very slow. If we measure a full VCSEL structure
under the same condition, it is thought that it takes about 10 h.
Fig. 3(a) and (b) shows that the Al and C profiles obtained by
the two energy sputtering method, respectively. The convoluted
and reconstructed profiles obtained by the MRI calculation are
also shown in Fig. 3. The Al measured depth profile has a
sufficient number of data points, and the individual layers in the
active region are resolved. In addition, the total measurement
time is approximately 90 min. However, the depth profile
shows a strong broadening of the interfaces.
The Al measured profile is fitted well by the MRI model with
following parameters: w ¼ 2:0 nm, s = 3.7 nm and l = 0.4 nm.
7277
This is surprising that the parameter of surface roughness, s, is
much larger. This result will be discussed later in this section.
The C measured profile was also analyzed by MRI model.
Three parameters obtained from the Al depth profile were used
for MRI calculation of the C depth profile. It is assumed that the
function of the original C distribution at the interface between C-
doped and undoped layers was an error function with a Gaussian
distribution [6]. The Gaussian standard deviation of an error
function can be varied during a fitting procedure. The convoluted
profile was found to fit well with the measured one at the standard
deviation of 0.3 nm. Thus, it seems that the diffusion of the C
atoms into the undoped GaAs wells is very small. Furthermore,
the values of C doping concentration in the modulation-doped
Al0.2Ga0.8As barriers were estimated to be 5.3  1018 cm
3 from
the original profile reconstructed by the MRI calculation. These
values were in good agreement with those obtained by measuring
the C-doped 200-nm-thick Al0.2Ga0.8As control sample grown
under the same growth condition.
Finally, the effect of two energy sputtering method on
surface roughness is investigated. Fig. 4 depicts the AFM
images of the crater bottoms after the 10-keV-sputtering and the
subsequent 1.5-keV-sputtering. The rapid sputtering using
10.0 keV high-energy ions results in a rougher surface with the
root-mean-square (rms) roughness of 2.76 nm, as seen in
Fig. 4(a), but decreased to 1.79 nm by the subsequent 1.5-keV-
sputtering (Fig. 4(b)). These AFM results indicate that the 10-
keV-sputtered surface recovers its smoothness by the 1.5-keV-
sputtering. However, this is rougher than that of the crater
bottoms after sputtering the DBR layer by 1.5-keV ions, i.e. rms
roughness of 1.03 nm (not shown). Therefore, it is believed that
the increase of roughness parameter, s, for the measured Al
profile in Fig. 3(a) is mainly due to the roughening of the initial
surface for the MQW measurement. If we can suppress the
surface roughness induced by DBR sputtering without
increasing the measurement time, it is thought that an MQW
depth profile with better depth resolution would be obtained.
5. Conclusion
We have analyzed an MQW structure in a VCSEL epitaxial
wafer using SIMS. In order to provide the depth profile of the
7278 S. Ootomo et al. / Applied Surface Science 252 (2006) 7275–7278
GaAs/Al0.2Ga0.8As MQW with a sufficient depth resolution
and a large number of data points in a practical measurement
time, we have used the two energy sputtering method based on
rapid high-energy sputtering for the top DBR mirror structure
and a subsequent low-energy sputtering for the MQW structure.
The MRI model was used to reconstruct the original in-depth
distribution of elements, assuming that the matrix effects such
as changes of ionization probability and sputtering rate
thorough an interface are small enough. The convoluted Al
and C curves are fitted well with the measured profiles. The
values of C concentration in modulation-doped Al0.2Ga0.8As
barrier layers are estimated to be 5.3  1018 cm
3 from the
reconstruction by the MRI calculation. These values are in good
agreement with the value obtained by measuring the thicker C-
doped Al0.2Ga0.8As control sample grown under the same
growth condition. It was also found that the surface roughness
induced by the high-energy sputtering degraded a depth
resolution of the MQW depth profile in deep region.
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