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 Nanotechnology

Nanotechnology 28 (2017) 105702 (8pp) https://doi.org/10.1088/1361-6528/aa596c

GaAsBi/GaAs multi-quantum well LED

grown by molecular beam epitaxy using a
two-substrate-temperature technique
Pallavi Kisan Patil1, Esperanza Luna2, Teruyoshi Matsuda1,
Kohki Yamada1, Keisuke Kamiya1, Fumitaro Ishikawa1 and
Satoshi Shimomura1
1
Graduate School of Science and Engineering, Ehime University, 3 Bunkyo-cho, Matsuyama, Ehime,
Japan
2
Paul-Drude-Institut für Festkörperelektronik, Hausvogteiplatz 5–7, D-10117, Berlin, Germany

E-mail: [email protected]

Received 7 December 2016, revised 11 January 2017

Accepted for publication 13 January 2017
Published 1 February 2017

Abstract
We report a GaAs0.96Bi0.04/GaAs multiple quantum well (MQW) light emitting diode (LED)
grown by molecular beam epitaxy using a two-substrate-temperature (TST) technique. In
particular, the QWs and the barriers in the intrinsic region were grown at the different
temperatures of TGaAsBi = 350 °C and TGaAs = 550 C, respectively. Investigations of the
microstructure using transmission electron microscopy (TEM) reveal homogeneous MQWs free
of extended defects. Furthermore, the local determination of the Bi distribution profile across the
MQWs region using TEM techniques confirm the uniform Bi distribution, while revealing a
slightly chemically graded GaAs-on-GaAsBi interface due to Bi surface segregation. Despite this
small broadening, we found that Bi segregation is significantly reduced (up to 18% reduction)
compared to previous reports on Bi segregation in GaAsBi/GaAs MQWs. Hence, the TST
procedure proves as a very efficient method to reduce Bi segregation and thus increase the
quality of the layers and interfaces. These improvements positively reflect in the optical
properties. Room temperature photoluminescence and electroluminescence (EL) at 1.23 μm
emission wavelength are successfully demonstrated using TST MQWs containing less Bi content
than in previous reports. Finally, LED fabricated using the present TST technique show current–
voltage (I–V ) curves with a forward voltage of 3.3 V at an injection current of 130 mA under
1.0 kA cm−2 current excitation. These results not only demonstrate that TST technique provides
optical device quality GaAsBi/GaAs MQWs but highlight the relevance of TST-based growth
techniques on the fabrication of future heterostructure devices based on dilute bismides.

Keywords: GaAsBi/GaAs multiple quantum wells, molecular beam epitaxy, two-substrate-

temperature technique, x-ray diffraction, TEM, optical properties

(Some figures may appear in colour only in the online journal)

1. Introduction (MQWs), is considered to be an attractive candidate for

GaAs-base optoelectronic devices [1–9]. The incorporation of
Group III–V compound semiconductors allowing access into a small amount of Bi leads to a large reduction in the bandgap
the 1.3–1.5 μm wavelength range are currently under intense and to an increase of the spin–orbit splitting energy of the
investigation because of the important role of lasers in optical alloy [10, 11] which will bring considerable merits to laser
fibre communications. Especially, bismuth (Bi) containing diodes (LDs) for optical communication based on this mat-
GaAs material, both as bulk and as multiple quantum wells erial system [12, 13]. Recently, room temperature (RT)

0957-4484/17/105702+08$33.00 1 © 2017 IOP Publishing Ltd Printed in the UK

Nanotechnology 28 (2017) 105702 P K Patil et al

photoluminescence (PL) emission at 1.52 μm has been

obtained from 30 nm thick GaAs0.892Bi0.108 layers grown at
310 °C–400 °C by molecular beam epitaxy (MBE) [14]. On
the other hand, the highest Bi composition reported to date is
22% in a 17 nm thick GaAsBi layer grown at 200 °C [15].
Due to its large miscibility gap, the growth of GaAsBi has
proven complicated, requiring very low growth temperatures
(<400 °C) in order to incorporate significant fractions of Bi
[15–20]. Therefore, the quality of GaAsBi is highly depen-
dent on the Bi composition, on the growth temperature [21]
and on the general growth conditions and procedure. Note
that the arsenic flux must also be accurately controlled as a
shortage of As may lead to surface roughness while an excess
Bi will cause droplets on the surface [21, 22].
Light emitting diode (LED) structures with 50 nm thick
GaAsBi and a Bi content of 1.8% [1] and 6% [7], respec-
tively, have previously been grown by MBE. They show RT Figure 1. XRD spectra with simulation fitting for p-i-n type
electroluminescence (EL) at 987 and 1200 nm, respectively. GaAsBi/GaAs MQWs on n-type (001) GaAs with 4.0% Bi content.
The insert shows the schematic illustration of the sample structure.
On the other hand, a GaAs0.978Bi0.022/(Al)GaAs single
quantum well laser, grown by metal-organic vapour phase
epitaxy (MOVPE), with an emission wavelength of 947 nm conventional effusion cells for Ga, As, Bi, Be and Si sources.
under electrical injection at RT was recently demonstrated The Bi and As4 beam equivalent pressure (BEP) were opti-
[5]. Furthermore, lasing operation at 1.2 μm by photoexcita- mized for higher Bi composition, in order to obtain a high
tion at RT was demonstrated with a 300–400 nm thick optical quality, resulting in BEPs of As4 and Bi of 1.0 ´ 10-5
GaAs0.941Bi0.059 layer grown on AlGaAs by MBE [6]. In and 5.4 ´ 10-7 mbar, respectively [22]. Eleven periods of
addition, there are reports on an hybrid MOVPE/MBE 8 nm GaAs0.96Bi0.04/GaAs (11.8 nm/11.8 nm) MQWs were grown
GaAs0.94Bi0.06/GaAs MQWs laser showing lasing operation on epiready n-type GaAs (001) substrates at a high growth
at 1.09 μm at 80 K [8]. Although GaAsBi laser and LED with rate of 1.2 μm h−1 using the TST technique. The MQW
good performances have already been demonstrated, some i-region was stacked between a 500 nm thick p-type GaAs
questions like extending the emission wavelengths and the layer doped with Be at 4 ´ 1018 cm−3 and a n-type GaAs
improvement of the optical properties still remain challen- layer doped with Si at 5 ´ 1017 cm−3, followed by another
ging. In addition, strain management is very important for the 100 nm n-type/p-type GaAs layer grown at 580 °C. A sche-
growth of active layers consisting of a GaAsBi single layer or matic illustration of the sample structure is shown in the insert
GaAsBi/(Al)GaAs alternating layers. Note that Bi atoms tend in figure 1. The substrate temperature of the GaAsBi layers,
to segregate during growth of GaAsBi and will then incor- TGaAsBi, was 350 °C and that of the GaAs layers, TGaAs, 550 °C.
porate into the (Al)GaAs barrier, therefore increasing the total The growth was interrupted for 5 min at the GaAs on GaAsBi
strain energy and altering the total thickness of the active interface to increase the substrate temperature from TGaAsBi to
layer [23]. Here we demonstrate that the growth of GaAsBi/ TGaAs while the growth was interrupted for 10 min at the
GaAs MQWs using a two-substrate-temperature (TST) tech- GaAsBi-on-GaAs interface in order to reduce the growth
nique during MBE growth, where the GaAs layer is grown at temperature of the Bi-containing layer [22, 24, 25]. The
a higher temperature than the GaAsBi layer to sig- substrate temperature was measured by a pyrometer calibrated
nificantlyreduce Bi segregation [22, 24]. The material grown using both InSb and Al melting points.
using the TST approach is of high optical device quality as The samples were characterized by high resolution x-ray
demonstrated by the successful realization of p-i-n diode diffraction (HRXRD) using a Phillips X’Pert Pro materials
structures based on GaAs0.96Bi0.04/GaAs MQWs with RT EL research diffractometer with an incident x-ray beam wave-
emission at 1.23 μm. A similar RT EL emission wavelength length of CuKα1, (λ = 0.154 06 nm). The Bi composition was
of 1.25 μm have already been achieved using GaAsBi/GaAs determined by curve fitting software (‘Epitaxy’, Panalytical)
MQWs with about 8% Bi [8]. Since our MQWs only contain assuming the lattice constant of zincblende structure GaBi is
4% Bi, this result implies that by using the TST technique we a=6.33 Å [10]. Furthermore, the sample microstructure,
are able to fabricate LEDs with EL emission at a wavelength was investigated by transmission electron microscopy (TEM),
similar to the longest reported so far (1.25 μm) while reducing where cross-sectional TEM foils were prepared in the [110]
the total Bi composition in the layer. ¯ ] projections using mechanical thinning followed by
and [110
Ar-ion milling. TEM investigations were carried out using a
Jeol JEM 3010 microscope operating at 300 kV equipped
2. Experimental details with a GATAN slow-scan CCD camera. Analysis of the
GaAsBi/GaAs MQWs region is based on g002 dark-field (DF)
The GaAsBi/GaAs MQWs discussed in this paper was pre- TEM micrographs, which is highly sensitive to variations in
pared by MBE using a VG-80H Mark-III system with the chemistry of the alloy in semiconductors with zincblende

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Nanotechnology 28 (2017) 105702 P K Patil et al

structure [23, 26]. The optical properties were investigated by about 1.9 nm, which is on the same order as the chemical
PL and EL spectroscopy. The signal was spectrally separated width in other III–V heterointerfaces. Furthermore, this abrupt
using a 30 cm monochromator and signals passed through a interface indicates that the growth interruption to reduce the
phase sensitive lock-in amplifier to eliminate the background temperature from TGaAs to TGaAsBi seems not to have a det-
noise from the measurements. For PL measurements, the rimental effect in the layers, at least in terms of interface
sample was excited with a continuous wave 630 nm wave- quality. On the other hand, the growth interruption to increase
length laser, which was focused onto the samples surface with the substrate temperature from TGaAsBi = 350 C to
a spot diameter of 200 μm at an excitation power of 3.8 mW. TGaAs = 550 C should enable desorbing out surface segre-
The RT EL spectra of the sample were measured for various gated Bi atoms from the GaAsBi layer and the growth of
injection current densities. A Keithley 2000 system was used GaAs at the higher TGaAs = 550 C should prevent the
to measure current–voltage (I–V ) characteristics. Finally, incorporation of Bi atoms into the GaAs layer, hence reducing
light output measurements were performed using an Anritsu segregation effects and improving the interface quality. We
ML910B optical power meter and an Advantest R6142 cur- find, however, that the GaAs-on-GaAsBi interface is slightly
rent generator with a ILXLightwave LDP-3811 power supply. broader than the GaAsBi-on-GaAs interface, with an interface
width (10%–90% criterion) of about 2.7 nm. Careful inspec-
tion of the experimental Bi profiles across individual QWs
3. Results (see figure 3) reveal that the profile resembles segregation
curves, with its characteristic profile and exponential-like
3.1. High resolution x-ray diffraction decaying tail. Note that recent experimental investigations of
the microstructure of GaAsBi/GaAs MQWs grown using
Experimental HRXRD spectra, together with simulation single-growth-temperature methods demonstrate that Bi seg-
curves best fitting the experimental measurements of the regation is significantly strong in this material system, even
GaAsBi/GaAs MQW LED structure are shown in figure 1. for MQWs grown at the low substrate temperature of 220 °C
The clear satellite peaks indicate good periodicity of the
[23, 27, 28]. We find that the experimental Bi profiles of
MQWs. From the simulation best fit of the data, we get that
MQWs grown using the TST method are still well described
the MQWs consist of 11.8 nm equally thick GaAs0.96Bi0.04
using Muraki’s phenomenological segregation model [29]. Bi
and GaAs layers. This result is consistent with our previous
segregation is small but still detectable. The segregation
investigation for the growth optimization [22]. Asymmetric
probability, R, can be evaluated from the fit of the exper-
reflection reciprocal space mapping measurements of the p-i-n
imental data to Muraki’s model, where the segregation
diode structure (not shown here) revealed that the MQWs
probability R defines the fraction of Bi atoms in the topmost
region is perfectly matched to the substrate [22].
layer that segregate into the next layer. The fit of several
profiles to Muraki’s model yield an average value of
3.2. Transmission electron microscopy R=0.79±0.01. The error is the standard deviation of the
Figure 2(a) shows a cross-sectional g002 dark field transmis- data. Hence, although Bi segregation is rather small, it is still
sion electron microscope (DFTEM) micrograph of the responsible for the broader GaAs-on-GaAsBi interface. An
GaAsBi/GaAs MQW LED sample grown by MBE using the important difference of these results with respect to previous
TST technique. Since g002 DFTEM imaging is chemically reports on GaAsBi/GaAs MQWs (most of them grown using
sensitive in semiconductors with zincblende structure, the a single substrate temperature) is that, even if Bi segregation
homogeneous intensity contrast, in particular at the bright is still present and not completely suppressed, the TST
areas corresponding to the GaAsBi MQWs, indicates a method proves very efficient in reducing Bi segregation,
homogeneous layer, without contrast (i.e. composition) which is significantly reduced, as much as ∼18%. The esti-
modulations [23]. No extended defects such as dislocations mation is based on the comparison of the segregation prob-
were observed within the MQWs. Quantitative chemical ability in MQWs grown at a similar temperature using a
determination from the analysis of the g002 diffracted intensity single-temperature method and TST. In particular, we com-
[26] yields [Bi] 3.9%. The quantitative determination of [Bi] pared the data reported in [23], where the MQWs show a very
relies on the analysis of the g002 diffracted intensity following strong Bi segregation (R=0.96, for TGaAsBi = TGaAs =
the procedure of Bithell and Stobbs [26], where we assume 370 C), with our TST MQWs, where R=0.79.
the substitutional incorporation of Bi at As sites, the validity Finally, as observed in the TEM micrographs of figures 2
of Vegard’s law and use the underlying GaAs barrier as a and 3, note that not all the QWs have the same thickness but
reference layer of known composition [23]. A representative there are slight differences in thickness among them. These
Bi distribution profile across several MQWs (i.e. along the slight deviations in QW thickness may explain the broadening
growth direction) is shown in figure 2(c). TEM observations of the XRD spectrum. Furthermore, any variation from the
over extended areas yield similar results. Figure 3 shows an nominal layer design (e.g. those arising from Bi segregation
enlarged Bi distribution profile extracted using the afore- or deviations from the intended thickness) will in turn alters
mentioned procedure. As observed, MQWs with abrupt the effective active region thickness and period and thus
GaAsBi-on-GaAs interfaces are obtained. Evaluation of the would induce corresponding deviations in the energy-band
GaAsBi-on-GaAs interface width (10%–90% criterion) yields structure and on the optoelectronic response.

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Nanotechnology 28 (2017) 105702 P K Patil et al

Figure 2. (a) Dark field g002 TEM image of GaAs0.962Bi0.38/GaAs MQWs grown using the two-substrate-temperature growth technique.
(b) Intensity linescan from the area marked in (a) from where the experimental Bi composition profile shown in (c) is obtained.

3.3. Optical properties 1.057 to 1.052 eV with increasing temperature from 14 to 50 K

and is accompanied with a broadening of the FWHM and a
3.3.1. Luminescence. The temperature-dependent PL of the
12 meV blueshift from 50 to 120 K. The peak of PL FWHM is
GaAs0.96Bi0.04/GaAs MQWs p-i-n diode sample from 10 to at 80–90 K in the region where the PL blueshift is observed. For
300 K is shown in figure 4 in logarithmic scale. The PL
temperatures above 120 K, the PL peak energy decreases
spectrum at 10 K in linear scale at the insert shows a sharp and
monotonically due to the energy band gap reduction with
single luminescence peak at 1.174 μm, with a full width at half
increasing temperature, while PL FWHM decreases and reaches
maximum (FWHM) of 64 meV [14]. With increasing
a local minimum at 180–210 K and increases again. These
temperature from 10 to 50 K, the PL peak shows a small but
results are consistent with those reported by Riordon et al
clear red shift from 1.174 to 1.181 μm. From 60 to 120 K, the
[1, 30]. At high temperature, the thermal distribution of carriers
peak moves to the shorter wave length side by 0.014 μm. With
and phonon scattering may cause broadening of the peak
further increase of the sample temperature, PL peak moves to
the longer wavelength side (∼1.23 μm at RT) due to the [8, 14]. The result indicates that the PL emission spectrum from
bandgap reduction [1, 22]. The peaks observed at 0.83–0.87 μm GaAsBi/GaAs MQW has two components, with lower and
are from GaAs layers. Figure 5 shows the temperature higher energy emissions. They are separated by 25 meV. The
dependence of the PL peak energy and FWHM of the p-i-n lower energy emission is from carrier recombination at
diode sample. A S-shape behaviour (redshift-blueshift-redshift) localized states [14]. The higher energy emission is from
is clearly seen in the temperature dependence of the PL peak carrier recombination at delocalized states, where we consider
energy together with the temperature dependent fundamental that the GaAsBi/GaAs system has a type I band configuration
energy gap expressed by the Varshni empirical formula, and the emission is from the type I transition [3, 30, 31]. If we
E0 (T ) = E0 (0) - aT 2 (b + T ) [14], where E0 (0) is the assume that the GaAsBi/GaAs system has a type II band
transition energy at 0 K, and a and b are known as the Varshni configuration with a conduction band offset value of ∼25 meV,
thermal coefficients, and E0 (0) = 1.277 eV, a = 0.44 as shown in the inset of figure 5, the lower energy emission
(meV K−1), and b = 430 K are determined by fitting. The might originate from the type II transition and the higher energy
value of b is much larger than that for GaAs (204 K) and emission from the type I transition [3]. Electrons and holes are
indicates a small temperature dependence of the emission separately located in the GaAs and GaAsBi layers, respectively,
wavelength. The PL peak energy decreases by 5 meV from at low temperatures. As the sample temperature increases, the

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Nanotechnology 28 (2017) 105702 P K Patil et al

Figure 3. (a) Dark field g002 TEM image of GaAs0.962Bi0.38/GaAs MQWs grown using the two-substrate-temperature growth technique.
(b) Intensity linescan from the area marked in (a) from where the experimental Bi composition profile shown in (c) is obtained. The
experimental Bi profiles data are fitted using Murakiʼs segregation model, from where the segregation probability R is extracted. Note that not
all the QWs have the same thickness but there are slight differences in thickness among them.

Figure 5. Temperature dependent PL peak energy with the Varshni

equation fitting (dashed line) and FWHM (open square) with respect
to temperature for GaAs0.96Bi0.04/GaAs MQWs. The main peak
Figure 4. Temperature dependence PL from GaAs0.96Bi0.04/GaAs shows an S-shaped shift with increasing temperature (solid circle).
MQWs. PL spectrum at 10 K with narrow 64 meV FWHM is shown The schematic band diagram is shown in the inset.
in the inset.
PL peak emission from the type I transition is dominant at
electrons are thermally activated and distribute in both the GaAs higher temperatures.
and GaAsBi layers. Generally, the type I transition probability The integrated PL intensity (IPL) of the GaAsBi MQW
is much higher than the type II transition probability. Hence, the emission is plotted in figure 6 as a function of temperature

5
Nanotechnology 28 (2017) 105702 P K Patil et al

Figure 7. Room temperature electroluminescence (EL) spectra for

Figure 6. Integrated PL (IPL) intensity as a function of 1000/T for GaAs0.96Bi0.04/GaAs MQWs LED for with various injection current
the GaAsBi-related emission in the GaAs0.96Bi0.04/GaAs MQWs. densities.
Activation energies are obtained from Arrhhenius plots.
mechanism of the EL is unaltered over the current range
reciprocal. It is clear that there are more than two activation [1, 3]. Even if the GaAs0.96Bi0.04/GaAs MQWs have a type II
energies. The data in figure 6 have been fitted with several band configuration, the type I transition is dominant at RT
different activation energies, each one determined by using because of the small conduction band offset as discussed in
Arrhenius formula to fit the data in a given temperature range. section 3.3 ‘Optical properties’. Actually, the optical
In the low temperature region from 10 to 40 K, the IPL properties of type II QWs are strongly dependent on the
intensity did not show a large change due to localization of band offset value [3, 30–32]. At maximum excitation current
excitons with activation energy of 0.79 meV. In the middle (I) of 130 mA, the LED shows 1.23 μm wavelength
temperature range from 40 to 120 K, the IPL intensity luminescence. Note that we have achieved this long
decreases exponentially with an activation energy of 11 meV. emission wavelength with MQWs containing 4% Bi as
In this temperature region, a blueshift of the PL peak and an compared to the GaAsBi/GaAs (50 nm/3 nm) LED with
increase-and-decrease of the PL FWHM was observed. 1.2 μm luminescence with 6% Bi-containing GaAsBi layers
Finally, an activation energy value of 46 meV is obtained reported by Richards et al [7]. The FWHM value is 34 meV
for the region at temperatures higher than 150 K [7]. With smaller than in that of the GaAsBi/GaAs (50 nm/3 nm) LED
increasing temperature, the carriers injected into the active [1, 7]. This longer emission and narrow line width indicate
layers were more thermally excited than those at low that the material has optical device quality and make the TST
temperature, resulting in a higher probability of escape from technique very promising for the fabrication of optical
localized states to delocalized states in MQWs. This leads to a devices based on bismides layers, such as LED and LDs
reduced recombination rate of electron–hole pairs in the with good performance with low threshold currents. In
MQWs because of nonradiative recombination centres particular, the TST technique yields MQWs with uniform Bi
[12, 30, 31]. composition and abrupt interfaces throughout the MQWs
region.
3.4. Light-emitting devices

3.4.1. Electroluminescence. EL spectra for a GaAsBi/GaAs 3.4.2. I–V and L–I characteristics. Figures 8(a) and (b) show
MQWs LED for various injection current densities I–V and L–I characteristics of the LED device. The increase in
(10–130 mA) at RT are shown in figure 7. The p-i-n type the voltage is obtained with increasing injection currents from
GaAsBi MQWs LED device consists of a 10 μm wide and 0 to 130 mA. At 100 mA the current density is 756 A cm−2.
1.30 mm long stripe p-electrode. Conventional standard The forward voltage at the highest injection current of
photolithographic technique was used for the LED 130 mA is 3.3 V and current density is 1.0 kA cm−2. The
fabrication process. The EL from the LED showed a sharp efficiency of this device has not been measured. Figure 8(b)
and single luminescence peak at 1.23 μm with narrow illustrates the typical output power of the fabricated LED.
FWHM of 100 meV, at the same wavelength emission as Light output versus current (L–I) characterization at
the RT PL peak. The weaker luminescence peak at 0.88 μm is continuous and pulse operation was carried out. Pulse
attributed to the GaAs cladding layer emission. Appearance of operation of LED shows better performance than light
strong emission with the increase in injection current indicates output from the edge of the sample under 1.0 kA cm−2
higher recombination. Since the shape of the spectrum current. The output power of LED increased with increasing
remains unchanged for the increasing current, the transition current at RT. Regarding the lighting mechanism, when the

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Nanotechnology 28 (2017) 105702 P K Patil et al

MQWs grown using the TST technique have optical device

quality and is advantageous as an active layer for longer
wavelength LEDs and LDs.

Acknowledgments

The author gratefully acknowledges the Ministry of Social

Justice and Welfare, India for Doctoral Fellowship (Pallavi
Patil, No. DSW/Edu/2012-2013/D-IV/564). E Luna
acknowledges M Matzeck and S Krauß for help with TEM
specimen preparation.

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