Journal of The Electrochemical Society, 154 共10兲 K87-K91 共2007兲 K87

0013-4651/2007/154共10兲/K87/5/$20.00 © The Electrochemical Society

The Effect of Nanoscale Protrusions on Field-Emission

Properties for GaN Nanowires
Kuo-Hao Lee,a Cheng-Da Shin,a In-Gann Chen,a,b,z and Bean-Jon Lic
a
Department of Material Science and Engineering, and bFrontier Material and Micro/NanoScience and
Technology Center, National Cheng Kung University, Tainan 701, Taiwan
c
Industrial Technology Research Institute, Material and Chemical Research Laboratories, Hsinchu 310,
Taiwan

GaN nanowires 共NWs兲 have been synthesized on platinum-coated silicon共111兲 substrates by the chemical vapor deposition 共CVD兲
method under different NH3 /H2 carrier gas–flow rate ratios. X-ray diffractometer and transmission electron microscope analyses
indicate that GaN NWs have wurtzite structures. Nanoscale protrusions with crystal orientation along the 关002兴 direction were
observed on the surface of GaN NWs grown under high H2 flow rate conditions. As compared to the field-emission result of GaN
NWs with smooth surfaces, GaN NWs with nanoscale protrusions exhibit a lower turn-on field of 8.5 V/␮m and a higher
field-enhancement factor of ␤ = 315. These nanoscale protrusions are believed to account for the enhancement of the field-
emission behaviors of GaN NWs.
© 2007 The Electrochemical Society. 关DOI: 10.1149/1.2766644兴 All rights reserved.

Manuscript submitted March 8, 2007; revised manuscript received June 5, 2007. Available electronically August 10, 2007.

Gallium nitride 共GaN兲 has a wide direct bandgap of 3.4 eV at a temperature of 950°C and total pressure of 260 Torr. The indi-
room temperature and is a popular semiconductor material with po- vidual growth parameters for each of the samples are tabulated in
tential applications in blue and UV light emission, high temperature, Table II.
and high power electronic devices.1,2 Recent efforts have been de- The crystal structure and phase of each of the samples were
voted to carbon nanotubes 共CNTs兲 and ZnO nanostructures to im- analyzed using the Rigaku D-Max-IV X-ray diffractometer 共XRD兲
prove the performance of conventional Spindt-type Mo field emit- and JEOL-2010F transmission electron microscope 共TEM兲. The
ters. Because Mo, CNTs, and ZnO have a work function around JEOL-JSM 7000F FE scanning electron microscope 共FE-SEM兲 was
4.5 eV, sharp needlelike nanostructures are required to enhance used to examine surface morphology. FE measurements were per-
electron emission with sufficient current density. GaN has attractive formed in a vacuum system at a pressure of 2 ⫻ 10−6 Torr. A volt-
properties as a material for field emitters, e.g., a lower work function age source was applied to a Pt sphere probe ball with a cross-
共4.1 eV兲 and stronger chemical and mechanical stability than those sectional area of 0.7 mm2 to collect emitted electrons from the
listed above. These properties make it a desired alternative material grounded GaN NW cathode. The anode-cathode distance was
for field emitters. Typical GaN nanostructure morphologies include 20 ␮m. Emission current was monitored by a Keithley 237.
nanowires 共NWs兲, nanorods, nanobelts, and nanotubes. Recently,
Results and Discussion
needlelike3 structures and quasi-aligned4 GaN NWs have been
grown and studies have shown that the sharp tip is responsible for Figure 1 shows SEM images of typical GaN NW morphologies
the enhancement of the field-emission 共FE兲 properties of NWs. The obtained at four different ratios of H2 /共NH3 + H2兲. The length of
resulting turn-on field is ⬃7.5 V/␮m for needlelike3 GaN NWs and these GaN NWs is several micrometers long and the diameter is
⬃7.0 V/␮m for quasi-aligned4 GaN NWs. In these studies, the elec- about 100 nm. GaN NWs are randomly orientated and intersect one
trons were emitted from the tip of the NW due to its high aspect another at various points. It is observed that at higher NH3 /H2 ratios
ratio. The FE characteristics of various GaN NWs created from dif-
ferent synthesizing methods are listed in Table I. All the GaN NWs
listed in this table were grown under a constant flow rate of NH3.
However, no study has ever been performed with different carrier
gases, such as H2. This report not only shows the effect of different
NH3 /H2 flow rate ratios on the growth and FE properties but also
demonstrates the ability to use platinum as the catalyst for GaN NW
growth of many other transition metals, such as Fe, Co, Ni, and Au.
Nanoscale protrusions with crystal orientation along the 关002兴 axis
were first observed on the surface of GaN NWs that were grown
under high H2 flow rate conditions. The correlation between the FE
behaviors and nanoscale protrusions were also explored in this re-
port.

Experimental
GaN NWs were grown by thermally reacting metallic Ga 共3 g兲
with different ratios of NH3 /H2 gases at 950°C for 30 min. In a
horizontal quartz-tube furnace with a diameter of 80 mm and length
of 120 cm, a platinum-coated 共thickness ⬃10 nm兲 Si共111兲 substrate
with an area of 1.5 cm2 was placed 5 cm downstream from the Ga
source. A series of samples were grown using different H2 /共NH3 Figure 1. SEM images of GaN NWs with different flow rate ratios of
+ H2兲 flow rate ratios with a constant total flow rate of 500 sccm at NH3 /H2. Each picture is magnified from the circle marker. The nanoscale
GaN protrusions can be observed, as marked by the arrows in 共c兲 and 共d兲,
and is shown schematically in inset of 共d兲. Protrusions with a typical size
smaller than 50 nm appear in both edges of the GaN NWs with a spacing of
z
E-mail: ingann@mail.ncku.edu.tw about 15–20 nm.
K88 Journal of The Electrochemical Society, 154 共10兲 K87-K91 共2007兲
Table I. FE characteristics of GaN NWs with different synthesized methods.

Effective
Growth emission area Turn-on field at 0.01 mA
Ref. Author Growth feature method 共mm2兲 共V/␮m兲 Value
7 Chen et al. GaN NWs CVD 12
13 CNT-encapsulated GaN CVD 5
28 Tereda et al. self-organized tip RIE
10 Kim et al. GaN NRs HVPE 0.5
9 Kang et al. GaN NRs HVPE 0.5
12 Kim et al. Ni catalyst CVD 7 7.4 555
14 Ni catalyst CVD 7 7.4 555
11 Luo et al. GaN nanobelts RF sputter 25 6.1 共at 0.1 uA/cm2兲 1600 and 750
23 Liu et al. P doped in GaN, Au catalyst CVD 5.1
3 Bicrystalline,Au catalyst CVD 7.5
4 Quais align, Au catalyst CVD 7.0
8 Ha et al. GaN NWs, Ni catalyst CVD 5 8.5 共at 0.1 uA/cm2兲 1170
15 Yamashita et al. GaN NRs PAMBE 0.49 1.25 共at 0.1 uA/cm2兲 1270 and 4960
16 Hasegawa et al. Polycrystalline GaN NRs PAMBE 6.4 共at 10 nA/cm2兲 280
17 Sugino et al. Smooth/roughed GaN surface Metallorganic CVD 12.4and21.6 61and120
29 Jang et al. GaN-BN nanocable CVD 7 1.4 共at 0.1 uA/cm2兲 1440

of NH3 /H2 = 400:100 and 300:200, as shown in Fig. 1a and b, re-
spectively, nearly all GaN NWs have smooth surfaces. As the
NH3 /H2 ratio decreases to 200:300, as shown in Fig. 1c, a small
amount of nanoscale protrusions appear on the GaN NWs. Further
decreases in the NH3 /H2 ratio to 100:400, as shown in Fig. 1d,
increase the amount of nanoscale protrusions. The typical size of the
protrusions are smaller than 50 nm and appear on both sides of the
NWs with a spacing of about 15–20 nm, marked by the arrows in
Fig. 1d.
Figure 2a shows the XRD results of the four different GaN NW
samples with different ratios of NH3 /H2. The diffraction peaks in
this spectrum can be indexed to the hexagonal structure of wurtzite
GaN phase and are in good agreement with the bulk GaN crystals
共JCPDS card No. 76-0703兲. No cubic-GaN peaks 关i.e., 共111兲 at
35.6°, 共200兲 at 41.3°, 共220兲 at 59.8°, and 共311兲 at 71.6°兴 and a very
low amount of impurities are observed in the XRD pattern. The
strong diffraction peaks relative to the background intensity indicate
the high purity of the wurtzite phase. The texture coefficient of the
共101兲 plane relative to the 共002兲 plane 共i.e., TC101−002兲 and the 共101兲
plane relative to the 共100兲 plane 共i.e., TC101−100兲 are shown in Fig.
2b to indicate the degree of preferred orientation of nanowires and
can be expressed as
I101 /I0101
TC101−002 = and TC101−100
I101 /I0101 + I002 /I0002
I101 /I0101
= radius 共or sharper兲 tip results in a higher local-field intensity at the
I101 /I101 + I100 /I0100
0
where I101, I002, and I100 are the diffraction peak intensities of the
共101兲, 共002兲, and 共100兲 planes, respectively. I0101, I0002, and I0100 are
the relative intensity values from the standard JCPDS file of ran-
domly oriented powder samples. If I002 /I0002
I101 /I0101, this indi-
cates that the 共002兲 plane orientation is preferred and results in
TC101−002 = 0. Similarly, TC101−002 = 0.5 would correspond to no
preferred orientations and TC101−002 = 1 indicates a preferred 共101兲
plane. The TC101−002 and TC101−100 values for the four different
samples with varying H2 /共NH3 + H2兲 ratios are shown in Fig. 2b
and Table II. It can be observed that as the H2 /共H2 + NH3兲 ratio
increases from 0.2 to 0.6, TC101−002 increases from 0.27 to 0.39,
whereas TC101−100 decreases from 0.495 to 0.47. At a H2 /共H2
+ NH3兲 ratio of 0.8, however, the TC101−002 is lowered slightly to a
value of 0.36 and TC101−100 is slightly increased to ⬃0.48. The
opposite trends between the TC101−002 and TC101−100 indicate that
different H2 /共H2 + NH3兲 ratios affect the preferred orientation of
GaN NWs in the growth process. It is known that the surface
energy5 of the 共101兲, 共002兲, and 共100兲 planes of wurtzite GaN are
125, 123, and 120 meV/Å2, respectively. A crystal plane with a
higher surface energy usually represents a higher density of dangling
bonds per unit area. Under high temperatures and H2 flow rate, the
highest surface-energy 共101兲 plane becomes the metastable plane
and transforms to a more stable 共002兲 plane. The effect of the H2
ambient for decreasing surface energy6 and the coexistance of 共101兲
and 共002兲 planes for GaN NWs were also observed.4 This growth
feature of 共002兲 planes is consistent with the SEM and TEM obser-
vations of Fig. 4 and are discussed in detail later. It is suggested that
the existence of H2 gas is responsible for the formation of the nanos-
cale protrusions with 共002兲 orientation.
It has been accepted that a nanowire or nanorod with a smaller
tip and therefore has an increased field-enhancement factor. As
shown in Table I, many different catalysts3,7,8 and growth methods,
such as hydride vapor phase epitaxy 共HVPE兲,9,10 radio frequency
共rf兲 sputtering,11 chemical vapor deposition 共CVD兲,7,12-14 and
plasma-assisted molecular beam epitaxy 共PAMBE兲15,16 have been

Table II. A list of GaN NW growth parameters, FE properties, and texture coefficient (TC101−002 and TC101−100) values derived from XRD for
each of the GaN NW samples. ␤ is the field-enhancement factor.a

Growth parameters FE results XRD results

NH3 H2 H2 共NH3,␤H2兲 Turn-on

Sample no. 共sccm兲 共sccm兲 ratio field 共V/␮m兲 TC101−002 TC101−100
a 400 100 0.2 12 247 0.271 0.496
b 300 200 0.4 13 105 0.316 0.491
c 200 300 0.6 19 131 0.393 0.468
d 100 400 0.8 8.5 315 0.361 0.477
a
The GaN NWs were grown in 950°C and total pressure of 260 Torr.
 Journal of The Electrochemical Society, 154 共10兲 K87-K91 共2007兲
Figure 2. 共Color online兲 共a兲 XRD patterns of GaN NWs grown in four
different flow rate ratios of NH3 /H2. All four samples show diffraction peaks
indexed as the hexagonal wurtzite structure. The top and bottom XRD pat-
terns are standard JCPDS files of hex-GaN and cubic GaN, respectively. 共b兲
Relationship between texture coefficients, e.g., TC101−002 and TC101−100, and
the H2 /共NH3 + H2兲 ratios.
K89
used to prepare sharp tipped and smooth-surface GaN NWs with a
turn-on field at ⬃10 V/␮m and a ␤ value of ⬃10.2,3 For GaN
epitaxy films,17 the as-grown smooth-surface films and the plasma-
treated rough-surface films have ␤ values reported to be 61 and 120,
respectively.
Figure 3a and b shows the FE measurements and corresponding
Flower–Nordheim 共F-N兲 plots of GaN NWs grown under different
NH3 /H2 ratios. As shown in Fig. 3a, different turn-on fields, which
are defined as the electrical field at which the emission current
=0.01 mA/cm2, are 12, 13, 19, and 8.5 V/␮m for the samples with
H2 /共H2 + NH3兲 ratios equal to 0.2, 0.4, 0.6, and 0.8, respectively.
The resulting data is listed in Table II. Compared with the values
from the literature as shown in Table I, the turn-on fields from this
study are of the same order of magnitude and fall within ⬃10 V/␮m
of the tabulated values. To calculate the field-enhancement factor
共␤兲, the F-N description of the FE for materials is expressed as
follows7
J=A
F2
␸
exp 冉
− B␾3/2
F
冊
where A = 0.014 and B = 6.8 ⫻ 10−9, F = ␤V/d with the voltage
共V兲 between the anode and cathode in volts, J 共A/cm2兲 is the current
density, ␸ 共eV兲 is the effective barrier height 共GaN = 4.1 eV兲, d共m兲
is the spacing between cathode 共GaN NWs兲 and anode 共Pt ball兲, and
␤ is the field-enhancement factor that depends on the emitter geom-
etry. The effective measurement area18 on the GaN NWs sample is
0.1 mm2. The straight lines of the F-N plots, as shown in Fig. 3b,
indicate electron emission from the GaN NWs following FE behav-
iors. Using the straight lines in the F-N plots, the field-enhancement
factor 共␤兲 of the four different GaN NWs were estimated to be 247,
105, 131, and 315, for H2 /共H2 + NH3兲 ratios of 0.2, 0.4, 0.6, and
0.8, respectively. These results are listed in Table II. The lowest
turn-on field of ⬃8.5 V/␮m and the highest field-enhancement fac-
tor 共␤兲 value of ⬃315 are both observed on the sample grown under
the highest H2 /共H2 + NH3兲 ratio of 0.8 with a large amount of
nanoscale protrusions on the GaN NWs, as shown in Fig. 1d.
Both the turn-on voltage and the field-enhancement factor 共␤兲
reveal that the GaN NWs with large amounts of nanoscale protru-
sions grown with the lowest NH3 /H2 ratio exhibit better FE charac-
teristics than those of the other samples. According to Fursey’s
observations,19 the nanoscale protrusions/roughness enhances FE
behaviors. This phenomenon has been observed on the tungsten tip
by the field ion microscope,20 in which different crystal orientations
result in different work functions21 and each protrusion can be a
local emission site.22 The randomly oriented nanoscale protrusions
shown in Fig. 1d can be treated as an array of fine emitters attached
to the surface of the GaN NWs and act as multiple FE sources with
better or comparable overall FE performance than that of a single
sharp tip. Similar results were also observed on NW samples with
rough surfaces.17,23-25
In the growth process of GaN NWs with nanoscale protrusions, it
is expected that the Ga vapor reacts with the N vapor, which is
decomposed from the NH3 at a high temperature of 950°C to form
the GaN structure. It has been reported that hydrogen has a higher
surface mobility and can stream easier and faster than the products
of GaN molecules.26 Therefore, hydrogen has a higher tendency to
occupy the surface defects on the substrate, which behave as hetero-
geneous GaN nucleation sites. When the GaN molecules encounter
the surface defects created by hydrogen, the large number of nucle-
ation sites enhances the probability of the random growth of GaN
crystals.27 Hence, the nanoscale GaN protrusions are observed when
GaN NWs are grown under high amounts of H2 carrier gas.
In Fig. 4a a typical low-magnification TEM image of GaN NWs
with protrusions is shown. The diameter of the NW is about 100 nm
with a protrusion size of about 50 nm. The inset in Fig. 4a displays
the corresponding diffraction pattern, which can be seen to have the
hexagonal wurtzite GaN structure with NWs along the 关1̄10兴 direc-
K90 Journal of The Electrochemical Society, 154 共10兲 K87-K91 共2007兲
tion and protrusions in the 关002兴 direction. The compositions of
NWs are displayed in the energy dispersive spectrum 共EDS兲 in Fig.
4b and can be noted to have a Ga-to-N ratio close to 1. Figure 4c
shows the high-resolution TEM 共HRTEM兲 image of a protrusion
from the GaN NW and Fig. 4d shows a magnified lattice image of
the region in circle A. The clear image illustrates that the protrusions
grow along the 关002兴 direction from the GaN NW.
Conclusion
This report demonstrates that platinum can be used as the cata-
lyst to grow GaN NWs as well as many other transition metals
through typical thermal CVD reactions of metallic Ga, NH3 and H2
carrier gas on platinum-coated Si substrate. SEM images indicate
Figure 3. 共Color online兲 共a兲 FE measure-
ments and 共b兲 corresponding F-N plots of
GaN NWs grown in different flow rate ra-
tios of NH3 /H2. The right inset in 共a兲
shows a magnified graph near the turn-on
field and the left inset in 共a兲 shows a sche-
matic of the FE measurement setup. The
distance between the Pt ball and the top of
GaN NWs 共dash line兲 is 20 ␮m. Both the
turn-on voltage and field-enhancement-
factor data are listed in Table II.
that the average diameter of the GaN NWs are about 100 nm with
random orientations. XRD and TEM diffraction patterns show that
GaN NWs have hexagonal wurtzite structures. In the sample grown
with a high H2 gas ratio, e.g., NH3 /H2 = 100:400, the high-surface-
energy 共101兲 plane of the GaN NWs evolves into nanoscale 共002兲
plane orientated protrusions to reduce the total surface energy. This
result is consistent with the XRD preferred-orientation analysis,
TEM, and SEM observations. HRTEM reveals that GaN NWs grow
along the 关1̄10兴 direction with nanoscale protrusions along the 关002兴
direction. With the study of the effect of different flow rate ratios of
NH3 /H2 on the GaN NWs growth and their corresponding FE prop-
 Journal of The Electrochemical Society, 154 共10兲 K87-K91 共2007兲
Figure 4. 共Color online兲 共a兲 TEM image of GaN NWs grown in NH3 /H2
= 100:400 shows 关1̄10兴 direction with a nanoscale protrusion in the 关002兴
direction. 共Inset兲 Electron diffraction pattern recorded from the circle mark.
共b兲 The EDS result of 共a兲 shows that the Ga-to-N ratio is close to 1. 共c兲
HRTEM image of a nanoscale protrusion and 共d兲 its corresponding HRTEM
image from circle A, which shows the orientation is 关002兴 direction.
erties, it is noted that both the lowest turn-on field of ⬃8.5 V/␮m
and the highest field-enhancement factor 共␤兲 value of ⬃315 is ob-
served on the sample grown under the highest H2 /共H2 + NH3兲 ratio
of 0.8. Additionally, the GaN NW grown under these conditions also
has a large amount of nanoscale protrusions on the surface, as
shown in Fig. 1d. These observations suggest that nanoscale GaN
protrusions can act as multiple FE sources that provide better overall
FE performance than that of a single sharp tip.
Acknowledgments
The authors thank the Center for Micro/Nano Technology Re-
search, Industrial Technology Research Institute, National Cheng
Kung University, Taiwan for support through equipment and coop-
eration.
K91
National Cheng Kung University assisted in meeting the publication
costs of this article.
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