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Synthesis, Morphology and Optical Properties of GaN and AlGaN Semiconductor

Nanostructures

Conference Paper · December 2013

DOI: 10.1063/1.4872988

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 Synthesis, morphology and optical properties of GaN and AlGaN semiconductor
nanostructures
B. Kuppulingam, Shubra Singh, and K. Baskar

Citation: AIP Conference Proceedings 1591, 1437 (2014); doi: 10.1063/1.4872988

View online: http://dx.doi.org/10.1063/1.4872988
View Table of Contents: http://scitation.aip.org/content/aip/proceeding/aipcp/1591?ver=pdfcov
Published by the AIP Publishing

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 Synthesis, Morphology and Optical Properties of GaN and
AlGaN Semiconductor Nanostructures
B. Kuppulingam, Shubra Singh and K. Baskar*

Crystal Growth Centre, Anna University, Chennai-600025, India

*E-mail:drbaskar2009@gmail.com

Abstract. Hexagonal Gallium Nitride (GaN) and Aluminum Gallium Nitride (AlGaN) nanoparticles were synthesized
by sol-gel method using Ethylene Diamine Tetra Acetic acid (EDTA) complex route. Powder X-ray diffraction (PXRD)
analysis confirms the hexagonal wurtzite structure of GaN and Al0.25Ga0.75N nanoparticles. Surface morphology and
elemental analysis were carried out by Scanning Electron Microscope (SEM) and Energy Dispersive X-ray spectroscopy
(EDX). The room temperature Photoluminescence (PL) study shows the near band edge emission for GaN at 3.35 eV
and at 3.59 eV for AlGaN nanoparticles. The Aluminum (Al) composition of 20% has been obtained from PL emission
around 345 nm.

Keywords: Sol-gel, PXRD, Gallium Nitride.

PACS: 61.46.Df, 78.66.Fd, 78.67.-n.

INTRODUCTION Al0.25Ga0.75N alloy nanoparticles by sol-gel method,

and its morphological and structural analysis.

The group III-nitrides system is attracting much

interest due to its direct band gap, which covers the
range from 0.7-6.2 eV and its commercial applications
such as green, blue and UV light emitting diodes
(LEDs), laser diodes, high-power and high temperature
electronic devices [1]. Among the ternary metal
nitrides growth of AlGaN have attracted interest in
recent years as bandgap can be tuned from 3.4 to 6.2
eV. AlGaN nanoparticles can be used in novel
electronic devices and studying of quantum
confinement effects, they can find possible application
in quantum lasers and single electron transistor [2].
There are few reports available for AlGaN
nanoparticles in the literature. Benaissa et al, have
reported the synthesis and luminescence of an AlGaN
nanoparticle imbedded in a polymer matrix which
consist of single-crystalline zinc blende structure [3].
Second report was on micro-raman investigation of
group III semiconductor nitride powder prepared by
pyrolysis of metal amide-imide precursors route [4].
The phonon states of AlGaN alloy nanocrystalline
solids has also been investigated prepared by
ammonothermal route [5]. Investigation on the surface
morphology and luminescence properties of AlGaN
nanoparticles are not widely available in the literature.
Here we report on the synthesis of hexagonal
EXPERIMENTAL DETAILS
AlGaN nanoparticles were synthesized by
nitridation of AlxGa(1-x)-EDTA complex at 900 ºC for 8
hrs. AlxGa(1-x)-EDTA.NH4 complex was prepared by
the mixture of GaCl3, AlCl3 and EDTA.NH4 in
aqueous solution at pH of 9. The solution was stirred
for more than 6 hrs and dried in an oven at 70 °C to
obtain (Al, Ga)-EDTA.NH4 complex. The AlxGa(1-x)-
EDTA complex was taken in an alumina boat and
placed inside the horizontal quartz tube reactor.
Nitrogen gas was allowed to pass through liquid
ammonia bubbler to carry NH3 and to react with the
complex during the synthesis. The complex was
nitridated at 900 ºC for 8 hrs to obtain AlGaN
nanoparticles. The synthesized AlGaN nanoparticles
were characterized by PXRD, SEM, EDX and PL.
RESULTS AND DISCUSSION
GaN and AlGaN were characterized using PAN
analytical XPERT-PRO X-ray diffractometer with Cu
Kα1 radiation at room temperature. Fig. 1(a,b) shows a
typical powder X-ray diffraction pattern of GaN and
AlGaN nanoparticles. Based on the standard reference
JCPDS (89-8624), all the observed peaks can be

Solid State Physics

AIP Conf. Proc. 1591, 1437-1439 (2014); doi: 10.1063/1.4872988
© 2014 AIP Publishing LLC 978-0-7354-1225-5/$30.00

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 indexed on the basis of a hexagonal unit cell of space
group P63mc, suggesting that the sample is single
phase without any impurity in good agreement with
reported values. The PXRD pattern of Al0.25Ga0.75N
sample shows 0.2º shift towards higher angle which is
due to incorporation of Al content in the GaN crystal
lattice. This confirms that the lattice parameter of
Al0.25Ga0.75N is lower than the pure GaN which is
consistent with literature. When small amount of Al
content was added to pure GaN the (002) peak
intensity decreases. All diffraction peaks were
broadened due to nano-sized effects. The crystallite
size was calculated by means of Debye-Scherrer
equation. The calculated crystalline size for GaN is
about 20 nm and for AlGaN it is about 13 nm. For
Al0.25Ga0.75N nanoparticle all the diffraction peaks
were broadened compared with GaN nanoparticle
which can be attributed to the decrease in crystallite
size.
FIGURE 1. PXRD pattern of a) pure GaN, b)
Al0.25Ga0.75N and EDX spectrum of c) pure GaN, d)
Al0.25Ga0.75N nanoparticles.
FIGURE 2. SEM image of (a,b) pure GaN
nanoparticles and (c,d) Al0.25Ga0.75N microrods.
EDX spectra for GaN and Al0.25Ga0.75N
nanoparticles were shown in Figure 1.(c,d)
respectively. EDX spectrum corresponding to GaN
nanoparticles shows only Ga and N with no other
elements. The Ga to N composition is measured to be
approximately equimolar ratio, whereas for
Al0.25Ga0.75N nanoparticles spectrum indicates the
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presence of Al, Ga, N and O elements. However the
presence of O peaks indicate the unavoidable surface
oxidation during synthesis process. Figure 2.(a,b)
shows SEM image of GaN nanoparticle synthesized at
900 ºC. The surface morphology of GaN showed
agglomerated flower like spherical shaped structures
consisting of nanoparticles. The average size of the
agglomerated spherical structures was about 800 nm.
Figure 2.(c,d) shows SEM image of AlGaN
nanoparticles synthesized at 900 ºC. The surface
morphology of nanoparticles is strongly dependent on
concentration of Al. When Al is incorporated in to
pure GaN the spherical nanoparticles changes to rod
like morphology.
Room-temperature photoluminescence spectra
were recorded using spectra physics HORIBA JOBIN
spectrometer Ar+ ion laser second harmonic generation
operated at 244 nm with a power of 0.2 W/cm2. Fig. 3a
shows the PL spectrum of pure GaN nanoparticle. The
near-band-edge emission was observed at 376 nm. The
wide and broad emission relative to the band edge
transition may result from surface states associated
with non-perfect surface termination or from defect
states caused by nitrogen deficiencies. Fig. 3b shows
the PL spectrum of Al0.25Ga0.75N nanoparticle. For
Al0.25Ga0.75N a shift in PL peak towards higher energy
is observed.
FIGURE 3. Photoluminescence spectra of a) GaN and
b) Al0.25Ga0.75N nanoparticles.
The bandgap of AlGaN vary linearly from the
bandgap values of the two binary ends such as GaN
and AlN. In general, if the variation of Al composition
is linear in Vegards law then Al composition and
bandgap of AlGaN can be calculated. The estimated
Al composition from the PL emission 345 nm yields
about 20%. Broadening of AlGaN peak due to oxygen
impurity present in the sample is evident from EDX
analysis. Wide broadening of PL emission may be due
to size dependent properties of as synthesized
nanoparticles and it can be improved by controlling the
experimental conditions such as concentration of the
precursor solutions, nitridation temperature and time.
 CONCLUSION
Semiconductor wurtzite GaN and AlGaN
nanoparticles were prepared by sol-gel method. The
crystalline structure was analyzed by XRD and the
chemical purity of as-synthesized nanoparticles was
confirmed by EDX measurement. The surface
morphology changes from spherical to rod like
nanostructure. Room temperature PL exhibits the
broad near band edge emission at 376 nm for GaN
nanoparticles and 345 nm for AlGaN nanoparticles.

REFERENCES

1. S. Nakamura, T. Mukai, M. Senoh, Appl. Phys. Lett.

64, 1687 (1994).
2. R. F. Service, Science 271, 920 (1996).
3. M. Benaissa, K.E. Gonsalves, S.P. Rangarajan, Appl.
Phys. Lett.71, 3685 (1997).
4. L. Jeffery, T. Waldek Zerda, Chem. Mater.11, 20-
22(1999).
5. Y.G. Cao, X.L. Chen, Y.C. Lan, J.Y. Xu, T. Xu and J.K.
Liang, J. Alloys and Compounds 309, L13-L15 (2000).

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