Ghazali et al.

Nanoscale Research Letters 2014, 9:685

http://www.nanoscalereslett.com/content/9/1/685

NANO EXPRESS Open Access

Synthesis of gallium nitride nanostructures by

nitridation of electrochemically deposited gallium
oxide on silicon substrate
Norizzawati Mohd Ghazali1, Kanji Yasui2 and Abdul Manaf Hashim1*

Abstract
Gallium nitride (GaN) nanostructures were successfully synthesized by the nitridation of the electrochemically deposited
gallium oxide (Ga2O3) through the utilization of a so-called ammoniating process. Ga2O3 nanostructures were firstly
deposited on Si substrate by a simple two-terminal electrochemical technique at a constant current density of 0.15
A/cm2 using a mixture of Ga2O3, HCl, NH4OH and H2O for 2 h. Then, the deposited Ga2O3 sample was ammoniated in
a horizontal quartz tube single zone furnace at various ammoniating times and temperatures. The complete nitridation
of Ga2O3 nanostructures at temperatures of 850°C and below was not observed even the ammoniating time was kept
up to 45 min. After the ammoniating process at temperature of 900°C for 15 min, several prominent diffraction peaks
correspond to hexagonal GaN (h-GaN) planes were detected, while no diffraction peak of Ga2O3 structure was detected,
suggesting a complete transformation of Ga2O3 to GaN. Thus, temperature seems to be a key parameter in a nitridation
process where the deoxidization rate of Ga2O3 to generate gaseous Ga2O increase with temperature. The growth
mechanism for the transformation of Ga2O3 to GaN was proposed and discussed. It was found that a complete
transformation can not be realized without a complete deoxidization of Ga2O3. A significant change of morphological
structures takes place after a complete transformation of Ga2O3 to GaN where the original nanorod structures of Ga2O3
diminish, and a new nanowire-like GaN structures appear. These results show that the presented method seems to be
promising in producing high-quality h-GaN nanostructures on Si.
Keywords: Electrochemical deposition; Gallium oxide; Gallium nitride; Nanostructure; Nitridation

Background reported by Wright et al. [13] and Huang Y et al. [14],

Gallium nitride (GaN) is a very hard, chemically and mech-
anically stable wide bandgap (3.4 eV) semiconductor mater-
ial with high heat capacity and thermal conductivity which
makes it suitable to be used for sensors [1-8], high power
electronic devices such as field-effect transistor (FET) [9]
and optoelectronic devices such as light-emitting diode
(LED) [10]. Up to this date, many techniques have been
explored to synthesize GaN nanostructures including nano-
wires, nanorods, nanodots and so forth since such low-
dimensional nanostructures are promising for increasing
the performance optoelectronic devices and the sensitivity
of sensors [11,12]. For example, GaN nanorods and nano-
wires have been applied for chemical sensing application as
* Correspondence: abdmanaf@utm.my
1
Malaysia-Japan International Institute of Technology, Universiti Teknologi
Malaysia, Jalan Semarak, 54100 Kuala Lumpur, Malaysia
Full list of author information is available at the end of the article
respectively, due to a large surface to volume ratio. GaN
nanodots have been used in photodetectors as reported by
Kumar et al. [15].
Recently, GaN on silicon carbide (SiC) or sapphire sub-
strate have been widely used for several specific electronic
applications. However, these substrates are expensive and
not available in large wafer size [16]. According to
Kukushkin et al., Si substrate seems to be more preferable
for the heterostructure growth of GaN due to the availa-
bility of Si in large wafer size, the low price of Si and the
maturity of Si-based technology [17]. In addition, the inte-
gration of GaN-based devices on Si platform seems to be
very attractive for the hybrid integration towards ‘More
than Moore’ technology [18]. Several vapor-phase tech-
niques have been reported for growing GaN nanostructures
directly on Si with high quality which include molecular
beam epitaxy (MBE) [19], metal-organic chemical vapor

© 2014 Ghazali et al.; licensee Springer. This is an Open Access article distributed under the terms of the Creative Commons
Attribution License (http://creativecommons.org/licenses/by/4.0), which permits unrestricted use, distribution, and reproduction
in any medium, provided the original work is properly credited.
Ghazali et al. Nanoscale Research Letters 2014, 9:685
http://www.nanoscalereslett.com/content/9/1/685
deposition (MOCVD) [20] and hydride vapor phase epitaxy
(HVPE) [21]. However, these vapor-phase techniques are
too expensive and their growth parameters are quite com-
plicated. In recent years, a transformation of the grown gal-
lium oxide (Ga2O3) structures on Si to GaN by a so-called
nitridation seems to be a simple method to create a GaN/
Si heterostructure [22]. Here, a nitridation is achieved by
annealing the Ga2O3 structures in ammonia gas. Li et al.
reported the repeatable transformation of the CVD-grown
GaN structures to Ga2O3 structures by an annealing in air
and back to GaN structures by an annealing in ammonia
[23]. Moreover, there are several studies reporting the
formation of GaN nanostructures by annealing the sput-
tered Ga2O3 layer on metal-coated Si substrates in ammo-
nia [24-27]. To our knowledge, the nitridation of the
electrochemically deposited Ga2O3 structures on bare Si
substrates to form GaN nanostructures without the assist-
ance of metal catalyzers does not appear in the published
literature.
Recently, we report the growth of Ga2O3 nanostructures
directly on Si without any assistance of metal catalyzer by
using a simple electrochemical deposition [28]. This liquid-
phase technique provides several advantages such as high
controllability of thickness and morphologies of Ga2O3
nanostructures due to a less number of growth parameters.
In this work, we investigate the formation of GaN nano-
structures by ammoniating the electrochemically deposited
β-Ga2O3 nanostructures on Si substrate. Up to this date,
no such similar work is reported where a combination of
liquid-phase and vapor-phase methods is utilized to form a
GaN/Si heterostructure. The effects of the ammoniating
times and temperatures were studied. The mechanism for
the growth of GaN was proposed and discussed.
Methods
In this study, the synthesis can be divided into two
major processes; i) a formation of Ga2O3 structures as
the ‘seed’ structures and ii) an ammoniating process to
transform Ga2O3 to be GaN. The deposition of Ga2O3
on Si (100) substrate (resistivity of 15 to 25 Ω · cm) was
carried out by a simple two-terminal electrochemical
process. In the electrochemical process, a mixture of
Ga2O3 (99.99%), HCl (36%), NH4OH (25%) and DI water
was used as an electrolyte [28]. Since Ga2O3 is insoluble
in water, HCl is added to dissolve Ga2O3. The prepar-
ation of electrolyte was done as follows. First, Ga2O3
was dissolved in 1.5 ml HCl. Then, 6.5 ml DI water was
added into the solution, followed by NH4OH as a pre-
cipitator, so that the pH of the mixture could be easily
adjusted. The deposition was done in electrolyte with
Ga2O3 molarity of 1.0 M (pH 6) at a constant current
density of 0.15 A/cm2. The Si substrate was cleaned with
modified RCA cleaning using ethanol, acetone and DI
water prior to the deposition in order to remove a native
Page 2 of 8
oxide layer. The growth time was fixed at 2 h. In this
electrochemical process, a platinum (Pt) wire was used
as an anode and Si substrate as a cathode. The sche-
matic of electrochemical setup is shown in Figure 1a.
After the deposition, the sample was immersed into the
DI water to remove any unwanted residue.
The electrochemically deposited Ga2O3 was ammoni-
ated in a quartz tube furnace as shown in Figure 1b, at
various times of 15, 30 and 45 min and temperatures of
800°C, 850°C and 900°C under a flow of ammonia (NH3)
gas of 100 sccm at atmospheric pressure. The timing
chart of ammoniating process is shown in Figure 1c. Be-
fore starting the ammoniating process, the sample was
put inside the quartz tube furnace and then the nitrogen
(N2) gas was purged for 10 min to flush out the air in
the quartz tube. After that, the temperature was in-
creased up to the setting temperatures, i.e. 800°C, 850°C
and 900°C from room temperature (RT) with a ramping
rate of 28°C/min. After reaching the setting temperature,
N2 gas was stopped and NH3 gas was introduced into
the furnace. The furnace was immediately switched off
upon reaching the setting ammoniating time. At the
same time, NH3 gas was immediately stopped and N2
gas was purged back into the furnace for 1 h to remove
the remaining NH3 gas during the cooling down process.
The ammoniated structures were characterized using field-
emission scanning electron microscopy (FESEM; Hitachi
SU8083, Hitachi, Ltd, Chiyoda-ku, Japan), energy disper-
sive X-ray (EDX) spectroscopy and X-ray diffraction (XRD;
Bruker D8 Advance, Bruker AXS, Inc., Yokohama-shi,
Japan).
Results and discussion
The nitridation of Ga2O3 to form GaN can be described
as follows. Firstly, NH3 decomposes to N2 and H2 at high
temperatures as illustrated by Equation 1 [29]. Then,
Ga2O3 structures are deoxidized by H2 to form gaseous
Ga2O as illustrated by Equation 2. Finally, GaN structure
is synthesized through the reaction of Ga2O and NH3.
2NH3 ðgÞ→N2 ðgÞ þ 3H2 ðgÞ ð1Þ
Ga2 O3 ðsÞ þ 2H2 ðgÞ→Ga2 OðgÞ þ 2H2 OðgÞ ð2Þ
Ga2 OðgÞ þ 2NH3 ðgÞ→2GaNðsÞ þ 2H2 ðgÞ þ H2 OðgÞ
ð3Þ
Figure 2a shows the top view FESEM images of the
electrochemically deposited Ga2O3 nanorods on Si sub-
strate before the ammoniating process was applied. The
lengths and diameters of the grown Ga2O3 nanorods
were estimated to be in the range of 1,000 to 4,200 nm
and 200 to 1,000 nm, respectively. It is noted that the
measured EDX spectra confirm the elements of Ga and
O, indicating the formation of Ga2O3 nanostructure.
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Figure 1 Schematic of (a) electrochemical setup, (b) nitridation set up and (c) growth timing chart.

Figure 2 Top view FESEM images of samples. (a) Before nitridation, (b) after 15 min, (c) after 30 min and (d) after 45 min of nitridation at 850°C.
Ghazali et al. Nanoscale Research Letters 2014, 9:685
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Figure 2b,c,d shows the top view FESEM images after
the ammoniating process at 850°C for 15, 30 and
45 min, respectively. In a glance, it can be seen that
there is no significant change of morphology taking
place even at long ammoniating time of 45 min. How-
ever, it can be seen that there is a slight change on the
surface of nanorods where the numbers of ‘hole’ in-
crease with the ammoniating time. From the EDX ana-
lysis as shown in Figure 3a, the atomic percentage of N
increases with ammoniating time while the atomic per-
centage of O decreases and the drastic changes seem to
take place after ammoniating time of 30 min. Figure 3b
shows the XRD spectra of samples before and after the
ammoniating process at 850°C for 15, 30 and 45 min
together with the XRD spectra of bare Si. In the bare Si,
five peaks were observed at 33.1°, 47.8°, 54.7°, 56.4° and
61.8° corresponding to Si(112), Si(002), Si(004), Si(113)
and Si(024), respectively. The as-grown Ga2O3 nanorods
show three prominent peaks at 31.8°, 46.2° and 55.5°
corresponding to β-Ga2O3(202), β-Ga2O3(112) and β-
Ga2O3(002), respectively. After being ammoniated for
15, 30 and 45 min, several peaks corresponding to
hexagonal GaN (h-GaN) planes were observed. However,
β-Ga2O3-related peaks were still detected in all grown
samples suggesting that β-Ga2O3 structures are not
completely being transformed to GaN. From these XRD
results, it can be said that an ammoniating time is not a
dominant parameter since the complete transformation
of Ga2O3 to GaN does not occur even at a long ammo-
niating time of 45 min.
Figure 4a,b,c,d shows the FESEM images for the as-
grown sample and the ammoniated samples at tempera-
tures of 800°C, 850°C and 900°C for 15 min, respectively.
It is noted here that β-Ga2O3 nanorods as shown in
Figure 4a were also grown using the similar procedures
and conditions with the samples shown in Figure 2
Figure 3 EDX analysis and XRD spectra. (a) Atomic percentage obtained from the EDX analysis and (b) XRD spectra of the samples nitridated
at 850°C with various nitridation times.
Page 4 of 8
where their properties are similar. After being ammoni-
ated at 800°C and 850°C, the general shape of the nano-
rods is still being preserved where no significant change in
their morphologies is observed, as shown in Figure 4b,c,
respectively. However, the same phenomenon with the
samples shown in Figure 2 was observed where the num-
bers of ‘hole’ structures in the nanorods increase with the
temperature. When the sample was further ammoniated
at 900°C, as shown in Figure 4d, the structures have chan-
ged from nanorods to nanowires with the estimated
lengths of 0.4 to 1.0 μm and diameters of 0.05 to 0.08 μm.
This result is consistent with the result reported by
Kim et al. where they claimed that the change of morph-
ology could be significantly affected by the ammoniating
temperature [30]. Figure 5a shows the EDX analysis for
the samples ammoniated at temperatures of 800°C, 850°C
and 900°C. It can be seen that the atomic percentage of N
increases with temperature while the atomic percentage of
O decreases. As shown in Figure 5a, the drastic change in
the atomic percentage seems to take place from 800°C to
850°C. Figure 5b shows the XRD spectra of the as-grown
samples and the ammoniated samples at temperatures of
800°C, 850°C and 900°C for 15 min together with the
XRD spectra of bare Si. After being ammoniated at 800°C,
850°C and 900°C, several h-GaN-related peaks were ob-
served. However, as expected, β-Ga2O3-related peaks are
being detected for the samples ammoniated at 800°C and
850°C, suggesting the incomplete transformation of β-
Ga2O3 to GaN. It can be simply said that the complete
transformation was achieved at ammoniating temperature
of 900°C where no β-Ga2O3-related peak was observed
except h-GaN peaks. The peaks related to GaN structures
were detected at 32.5°, 34.6°, 36.9° and 58.0° corresponding
to h-GaN(010), h-GaN(002), h-GaN(011) and h-GaN
(110), respectively. The obtained results show a similar
tendency with the results reported by Li et al. [31] where
Ghazali et al. Nanoscale Research Letters 2014, 9:685 Page 5 of 8
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Figure 4 Top view FESEM images of samples. (a) Before nitridation, (b) after nitridation at 800°C, (c) after nitridation at 850°C and (d) after
nitridation at 900°C for 15 min.

the complete transformed GaN with hexagonal wurtzite
structure was obtained at a temperature of 900°C. It is
noted that from the EDX analysis, the atomic percentage
of O is not zero in the sample of 900°C. It is speculated
that the detected O element is contributed by a native
oxide layer in the sample after being exposed to air ambi-
ent. From these XRD results, it can be said that an ammo-
niating temperature is the key parameter in producing the
complete transformation of Ga2O3 to GaN since it takes
only a short ammoniating time of 15 min.
Based on the obtained morphological and structural
properties, the reaction mechanism for the transformation
of Ga2O3 to GaN under a flow of ammonia with the
dependence of temperatures is proposed and discussed. In
principle, as shown by Equation 1, with the increase of
temperature, the decomposition rate of NH3 should be in-
creased, resulting to the generation of a high density of H2.
Then, this leads to the higher deoxidization or vaporization
rate of Ga2O3 structures to form gaseous Ga2O, as illus-
trated by Equation 2 [32]. Finally, this situation would in-
crease the reaction of gaseous Ga2O and NH3 to promote
the formation of a GaN structure. This means that the
transformation of Ga2O3 to GaN does not proceed without
the deoxidation or vaporization of Ga2O3 or, in other

Figure 5 EDX analysis and XRD spectra. (a) Atomic percentage obtained from the EDX analysis and (b) XRD spectra of the samples nitridated
at various temperatures for 15 min.
Ghazali et al. Nanoscale Research Letters 2014, 9:685
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words, without the existence of gaseous Ga2O. Due to such
deoxidization and reaction activities, it is speculated that
the original morphological structure of Ga2O3 will be
diminished and a new morphological structure of GaN will
be formed. As shown in Figure 4b, the SEM image of the
ammoniated structure at temperature of 800°C shows no
significant change of the morphology as compared to the
unammoniated structure shown in Figure 4a. This seems
to show that the temperature of 800°C is considerably low
for the aggressive deoxidization or vaporization of Ga2O3
to take place, resulting to low reaction of gaseous Ga2O
and NH3 to form GaN. This also agrees with the XRD ana-
lysis as shown in Figure 5b where the sample ammoniated
at temperature of 800°C contains a mixture of Ga2O3 and
GaN structures. Figure 6a illustrates the growth mechan-
ism for the temperature of 800°C. When the temperature
is increased to 850°C, the morphology of the ammoniated
structure shows a slight change where the numbers of
‘hole’ structures seem to be increased as shown in Figure 4c.
It can be said that the deoxidization or vaporization rate of
Ga2O3 slightly increases to form gaseous Ga2O. However,
Figure 6 Proposed growth mechanism for the transformation Ga2O3 to GaN. At ammoniating temperatures of (a) 800°C, (b) 850°C and
(c) 900°C.
Page 6 of 8
since the original structure of Ga2O3 does not diminish
and the XRD spectra also shows a mixture of Ga2O3 and
GaN, it can be said that the temperature of 850°C is still
not favorable to drastically increase the density of gaseous
Ga2O to continuously react with NH3 to form a GaN
structure. Figure 6b illustrates the growth mechanism for
the temperature of 850°C. At high temperature of 900°C,
as shown in Figure 4d, it can be seen that the original
nanorod structure of Ga2O3 has diminished and a new
structure in the form of nanowire-like structure has been
produced. It can be said that temperature of 900°C seems
to be high enough to realize a complete deoxidization of
Ga2O3 to generate a high density of gaseous Ga2O. Thus,
the reaction of gaseous Ga2O and NH3 seems to be well
promoted at such condition to form GaN nanowires. It is
noteworthy that during the ammoniating process at
temperature of 900°C, white ‘cloudy’ ambient was observed
in the furnace which seems to indicate the aggressive deox-
idization of Ga2O3 to form Ga2O gaseous. After ammoni-
ating process, it was found that the original white colour of
the as-grown Ga2O3 diminished and new structures in
Ghazali et al. Nanoscale Research Letters 2014, 9:685
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light yellow colour appeared. The XRD spectra as shown in
Figure 5b reveals that the detected peaks belong only to the
structures of GaN. It can be said that the temperature of
900°C is favorable to drastically increase the deoxidization
rate of Ga2O3 to generate gaseous Ga2O to continuously
react with NH3 to form GaN with new morphological
nanostructures.
Conclusions
The nitridation of the electrochemically grown Ga2O3
nanostructures to form GaN nanostructures on Si plat-
form have been studied by varying the ammoniating times
and temperatures. The complete transformation of Ga2O3
nanorods to h-GaN nanowires was achieved at 900°C with
a short ammoniating time of 15 min. The obtained results
suggest that the effect of the ammoniating temperature in
realizing a complete transformation is more prominent
than the ammoniating time. Form the proposed growth
mechanism, it was found that a complete transformation
to GaN nanostructures can not be realized without a
complete deoxidization of Ga2O3. In a complete trans-
formation process, it seems to show the occurence of
morphological change. The presented method seems to be
promising for the formation of h-GaN nanostructures on
Si for the applications in sensing and optoelectronics.
Competing interests
The authors declare that they have no competing interests.
Authors’ contributions
NMG designed and performed the experiments, participated in the data
analysis and prepared the manuscripts. KY participated in the nitridation
process and revision of manuscript. AMH conceived the study, designed the
experiments, participated in the data analysis and revised the manuscript. All
authors read and approved the final manuscript.
Acknowledgements
The authors would like to thank for the supports provided by MIMOS Berhad
and Universiti Sains Malaysia. N. M. Ghazali thanks Malaysia-Japan International
Institute of Technology (MJIIT) for the scholarship. This work was supported by
Nippon Sheet Glass Corp, Hitachi Foundation, MJIIT, universiti Teknologi
Malaysia, Malaysian Ministry of Education and Malaysian Ministry of Science,
Technology and Innovation through various research grants.
Author details
1
Malaysia-Japan International Institute of Technology, Universiti Teknologi
Malaysia, Jalan Semarak, 54100 Kuala Lumpur, Malaysia. 2Department of
Electrical Engineering, Nagaoka University of Technology,
Kamitomioka-machi, Nagaoka, Niigata 940-2137, Japan.
Received: 24 October 2014 Accepted: 9 December 2014
Published: 18 December 2014
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doi:10.1186/1556-276X-9-685
Cite this article as: Ghazali et al.: Synthesis of gallium nitride
nanostructures by nitridation of electrochemically deposited gallium
oxide on silicon substrate. Nanoscale Research Letters 2014 9:685.

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