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On the growth and electrical characterization of CuO nanowires by thermal oxidation

A. M. B. Gonalves, L. C. Campos, A. S. Ferlauto, and R. G. Lacerda

Citation: Journal of Applied Physics 106, 034303 (2009); doi: 10.1063/1.3187833

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On the growth and electrical characterization of CuO nanowires

by thermal oxidation
A. M. B. Gonalves,a L. C. Campos, A. S. Ferlauto, and R. G. Lacerda
Departamento de Fsica, Laboratrio de Nanomateriais, Universidade Federal de Minas Gerais,
Antonio Carlos, 6627, 30123-970 Belo Horizonte, Minas Gerais, Brazil
Received 4 March 2009; accepted 29 June 2009; published online 5 August 2009
We present a detailed study on the growth process of cupric oxide CuO nanowires by thermal
oxidation. The morphology of nanowires, obtained at different oxidation temperatures and times,
was determined. The diameter of nanowires was found to depend linear on temperature whereas the
time dependence of their length is modeled by a parabolic law. The results suggest that CuO
nanowires are formed as a result of the competition between grain boundary and lattice diffusion of
Cu atoms across a Cu2O layer. Electrical characterization of the nanowires was also performed. A
field effect transistor was produced with an isolated nanowire showing p-type characteristics. The
resistivity, mobility, and density of carriers were calculated. Nanowire growth by thermal oxidation
is very simple and has great potential to be used for large scale production; this opens possibilities
for various kinds of application. 2009 American Institute of Physics. DOI: 10.1063/1.3187833

I. INTRODUCTION for 100 s, followed by rinsing with de-ionized water and

drying by N2 flow. The copper pieces were loaded in the
One-dimensional 1D structures, such as nanorods and
center of a horizontal quartz tube, which was then placed in
nanowires NWs, have become important building blocks of
a conventional tube furnace. The growth process occurs un-
nanodevices and integrated nanosystems.1 A wide variety of
der atmospheric pressure in air. Initially, we study the influ-
nanostructured semiconductors materials Si, Ge, and III-V
ence of the temperature on the growth of CuO NWs; six
semiconductors and oxides CuxO, ZnO, TiO2, SnO2, etc.
samples have been prepared at temperatures of 300, 400,
have been the focus of intense studies in the past years. Dif-
500, 600, 700, and 800 C. For temperatures fixed at 400
ferent approaches, such as vapor-liquid-solid, vapor-solid
and 600 C we also studied the influence of time on the
VS growth, template mediated growth methods, among
growth; six samples for each temperature were prepared at
others, have been used for the preparation of these 1D
deposition times of 10 and 30 min and 1, 3, 10, and 18 h.
nanostructures.24 In particular, cupric oxide CuO is a
Sample morphology was observed by scanning electron
monoclinic structure p-type semiconductor of narrow band
microscopy SEM on a JEOL-840A scanning electron mi-
gap 1.2 eV5 with promising potential for applications in
croscope using an accelerating voltage of 20 kV. The crystal
catalysis,6 gas and glucose sensors,711 field emission,12,13
structure and the composition of the as synthesized CuO
and field effect transistors FETs.11,14 CuO has complex
NWs as grow were analyzed using RIGAKU-Geigerflex
magnetic phases and forms the basis of several high-Tc
x-ray diffractometer operated at 40 kV with Cu K radiation
superconductors.15,16 CuO 1D nanostructures have also been
= 0.1542 nm. Measurements of isolated NWs were per-
grown by various methods such as chemical routes,17,18 tem-
formed using synchrotron radiation X-ray diffraction XRD
plate ways,19,20 and by eletrospinning techniques.14 Recently,
= 0.1542 nm on the beam line XRD1 of the Brazilian
various groups report the growth via a thermal oxidation
Synchrotron Light Laboratory LNLS. Raman spectroscopy
technique2125 which is extremely simple and has the poten-
were conducted using a Jobin Yvon Renishaw Raman sys-
tial to be adapted for large scale quantities. However, a clear
tem 3000 with an Olympus microscope BTH2, and a 100
understanding of the growth process is still lacking and very
objective spectrometer equipped with a cooled charge
little is known about the electrical properties of these nano-
coupled device detector. The spectral excitation was pro-
structures. In this work, we present a systematic study on the
vided by an argon laser 647.1 nm with a power of 2.3 mW.
growth and electrical characterization of the CuO NWs by
Electrical measurements were performed using a Keithley
thermal oxidation of copper foils in air.
237 high voltage measure unit for current-voltage curves. A
Keithley 230 programmable voltage source was used for the
II. EXPERIMENTAL application of the gate voltage. The measurements were re-
alized in ambient atmosphere.
Commercial copper foils 99.9% purity, 0.2 mm thick-
ness of about 5 5 mm2 and wires 99.9% purity, 0.5 mm
of diameter were used as the starting material. The copper
pieces were cleaned by HCl 37% under an ultrasonic bath Figure 1 depicts SEM micrographs of CuO NWs grown
at different temperatures. For 3 h of thermal oxidation, a
Author to whom correspondence should be addressed. Electronic mail: large temperature window between 400 and 700 C of CuO NW growth Figs. 1b1e can be observed, whereas

0021-8979/2009/1063/034303/5/$25.00 106, 034303-1 2009 American Institute of Physics

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034303-2 Gonalves et al. J. Appl. Phys. 106, 034303 2009

FIG. 1. SEM images of CuO NWs growth for 3 h at different temperatures.

a 300 C, b 400 C, c 500 C, d 600 C, e 700 C, and f
800 C. The inset in b shows a cross-sectional view of the same sample.

under 300 C and above 800 C Figs. 1a and 1f, respec-

tively no growth occurred. The appearance of NWs in the
temperature range between 400 and 700 C was reported by
other research groups.2124 It is also to be noted that the CuO
NWs grow perpendicular to the surface of the sample and FIG. 3. Color online a XRD pattern and b Raman spectrum of isolated
CuO NWs.
above of an oxide layer see the inset in Fig. 1. Further
analysis of the CuO NW morphology shows that their diam-
eter increases with increasing oxidation temperature from oxidation times. Similar results were obtained for the series
30 to about 250 nm, as depicted in Fig. 2. Figure 3 shows grown at 600 C. It is to be noted that by fixing the growth
the XRD pattern and Raman spectrum of isolated CuO NWs. temperature and varying the growth time, the average NW
By isolated we mean that the CuO NWs were removed from diameter remains roughly constant whereas the average
the oxide layer depicted in the inset of Fig. 1. Comparing the length increases with time. Figure 5 shows in detail the de-
XRD results Fig. 3a with the database for the CuO mono- pendence of the average NW length on the oxidation time for
clinic phase, all the peaks positions matched. Raman spec- the two investigated temperatures, as determined from the
trum Fig. 3b of the as-prepared CuO NWs shows three analysis of the SEM images. It is well known that similar to
peaks at 296, 345, and 630 cm1. In comparison with the several oxides, copper oxide formation follows a parabolic
vibrational spectrum of single crystal of CuO,26 the Raman law, i.e., d2 = k t, where d is the thickness of oxide layer, k is
peaks are also correct. We can assign the peak at 296 cm1 growth rate, and t is the time.27 The solid lines in Fig. 5
to the Ag mode, and the peaks at 345 and 630 cm1 to the Bg represent adjusts to the experimental data using such expres-
modes. These results clarify that the NWs are composed of sion. The obtained values for the growth rate constant, k,
CuO only and do not have a mixture of CuO and Cu2O were 1.7 0.5 1014 and 7.3 0.5 1012 m2 / min for
phases. T = 400 and 600 C, respectively. The fits suggest that NW
For a better understanding of the growth process, we growth can be explained by the same mechanisms that con-
realized a second series varying the oxidation time at two
fixed temperatures 400 and 600 C. Figure 4 presents SEM
micrographs for CuO NWs grown at 400 C for different

FIG. 4. SEM images of CuO NWs obtained from different oxidation times
FIG. 2. Color online Average diameter of CuO NWs as a function of and fixed temperature 400 C. a 10 min, b 30 min, c 1 h, d 3 h, e
oxidation temperature. The line is a guide to the eye. 10 h, and f 18 h.
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034303-3 Gonalves et al. J. Appl. Phys. 106, 034303 2009

FIG. 5. Color online Average NW length as a function time for oxidations

performed at 400 triangles and 600 C squares. The solid lines are fits of
the experimental data using a parabolic function. The y-axis is in log scale to FIG. 6. Color online Scheme of proposed model for the growth of CuO
facilitate the view of both data sets. NWs by thermal oxidation right. Cross-sectional view of an oxide layer
grown at 400 C showing the two oxide layers and the NWs. The scale
was detached from the remaining Cu foil due to stress.
trol the formation of oxide films, i.e., its rate-limiting step is
mass transport via diffusion. It is also interesting to observe been set forth more recently.23 In contrast, recent papers have
that the growth rate of NWs for 600 C is higher than the proposed very different mechanisms based on the evapora-
growth rate of the ones deposited at 400 C, which indicates tion and recondensation of oxide species VS models,4 how-
that the growth is a thermally activated process. ever, such models can be disregarded because in order to
The growth mechanism of CuO NWs via thermal oxida- generate the growth rates observed, the partial pressures of
tion is not completely established in literature.2124 Since we the precursor species would have to be much larger than the
observed that CuO NW growth kinetics is qualitatively simi- expected ones.25
lar to copper oxidation kinetics it is natural to apply the In this sense, we propose that the CuO NWs are formed
accumulated knowledge on such extensively studied phe- as a result of the rapid, short-circuit diffusion of the Cu ions
nomena to the understanding of the NW growth. In addition, across grain boundaries and/or defects in a underlying Cu2O
other metals such as iron and zinc can also form oxide NWs layer. A schematic of the proposed model is shown in Fig. 6.
when oxidized,28,29 suggesting that there should be general Initially a Cu2O layer is formed, and due to the large com-
mechanism for whisker appearance during metal oxidation. pressive stress such layer is highly porous and defective.25
The thermal oxidation of Cu depends sensibly on param- Since Cu2O formation happens at the oxide/air interface, for
eters such as purity, oxidizing atmosphere, and temperature. further oxidation to occur, Cu atoms find two pathways to
Moreover, usually the oxidation process results in a two- reach the growing interface: lattice and grain-boundary dif-
layer microstructure consisting of a Cu-rich Cu2O phase in fusion. The migration via the first pathway gives rise to the
contact with the Cu and a topmost CuO layer. In a recent continuous increase in the Cu2O oxide layer, whereas the
review by Zhu et al.,30 the effect of the temperature on the second results in the formation of the NWs. These ideas
Cu oxide formation was summarized into the following pic- share similarities with the model proposed recently for CuO
ture. Growth rate usually follows the well-known parabolic and Fe2O3 NW formation.21,25,28 Chopra et al. studied the
relation associated to diffusion limited processes, commonly growth mechanism of CuO NWs from thin film multilayer
observed in metal oxidation; however, the dominant diffu- mesa structure. They measured the time evolution of the
sion mechanism depends on temperature. For temperatures NW length and compared to detailed kinetics and thermody-
above 800 900 C, mainly Cu2O is formed and the outward namics calculations. They conclude that the only possible
lattice diffusion of Cu is the rate-limiting step. As the tem- mechanism for NW growth is via grain-boundary diffusion;
perature is lowered, there is an intermediated temperature however, they claim that growth results from the oxygen ion
range between 600 and 900 C wherein grain-boundary indiffusion across a generic mixed-phase Cu2O / CuO layer.
diffusion or defect-mediated diffusion also becomes relevant. In contrast, we believe that the rate-limiting step is the Cu
The formation of a topmost thinner layer of CuO over the diffusion across the Cu2O layer. Oxygen might be diffusing
Cu2O layers is usually observed as well. For temperatures across the topmost porous CuO layer, but since this layer is
below 500 C, the grain-boundary diffusion becomes domi- usually much thinner than the Cu2O layer,30 this step should
nant. not be the limiting one. In fact, cross-sectional SEM analysis
Since early works in 1950s and 1960s, many research of the oxide layers by Zhu et al.33 clearly demonstrates that
groups studying copper oxidation have observed whiskers at the base of the NWs is located in the interface between two
the surface of the oxide layer.31,32 Whiskers or NWs usu- oxide layers. Accordingly, the SEM picture presented in Fig.
ally appear for oxidation temperatures ranging between 400 6 also indicates a similar feature; however, the grain bound-
and 700 C31,32 and are usually accompanied by a porous aries and, therefore, the NW bases are not clearly distin-
CuO layer. Initially, it was proposed that the driving force for guished because no corrosion to reveal the grain boundaries
whisker formation was the high compressive stress in the was performed. This model is further supported by a recent
oxide scales resulting from the large difference in the molar work in which a comparative study is made between the
volumes of the metal and oxides.32 Similar interpretation has oxidation of coarse and nanosized grained copper, wherein it
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034303-4 Gonalves et al. J. Appl. Phys. 106, 034303 2009

was observed that the NW formation is greatly enhanced in

the nanocrystalline copper due to the larger number of grain
boundaries.34 In addition, an enhanced solubility of oxygen
on the nanocrystalline Cu was observed suggesting that oxy-
gen indiffusion might play an important role in Cu
Now, we discuss how the proposed model can describe
the obtained results. First, the time dependence of the NW
length, observed in Fig. 5 for 400 and 600 C, can be di-
rectly attributed to grain-boundary diffusion of Cu ions to-
ward the Cu2O / CuO interface parabolic diffusion law27
since the variations in the NW densities and diameters during
growth are small. The model also explains the changes in the
morphology of the NWs as a function of the oxidation tem-
perature as observed in Fig. 1. The morphology of the NW
layer will be, in fact, determined by the microstructure of
the underlying Cu2O layer because it is within this interme-
diate layer that the short-circuit diffusion of Cu atoms will
take place. In turn, the microstructure of the Cu2O layer is
affected by several variables such as the original microstruc-
ture of the Cu, presence of impurities, accumulated stress,
and most importantly, temperature. For low temperature due
to the low mobilities, the Cu2O layer will have small and FIG. 7. Color online a I vs Vsd curves at different gate voltages. b I vs
defective grains, and thus the density of grain boundaries Vg curve for a fixed 5 Vsd voltage. This result reveals an intrinsic p-type
behavior of CuO NW. The inset shows an isolated CuO NW between two
will be high. Consequently, a high density of thin NWs is
observed for 400 C Fig. 1b. As temperature is increased,
thermally induced grain growth within the recently formed
Cu2O layer will result in a reduction in the number of short- stance, a demonstration of a field effect response was re-
circuit diffusion paths. As a result NW density decreases as ported on CuO nanofiber14 and NW.11 In these works, a
p-type behavior and a weaker dependence of the conductiv-
temperature increases, as seen in the sequence of SEM im-
ity on gate voltage were observed. Compared to our results
ages of Fig. 1. Moreover, it is well documented that for tem-
they are similar. The mobility of the carriers can be estimated
peratures greater than 800 C, Cu oxidation is dominated by
from the FET transconductance,36 gm = Isd / VG
lattice diffusion of Cu ions, being negligible the relative con-
= CoxVsd / L , where is the carrier mobility. The capaci-
tribution of diffusion via grain boundaries or extended
tance is given by Cox = 20rL / cosh1t / R,37 where r is
defects.30 This explains the absence of NWs for oxidations
dielectric constant of SiO2, t is the thickness of dielectric, L
at high temperatures Fig. 1f.21 For temperatures below
is the length, and R is radius of CuO NW. The mobility
400 C, the growth rate is significantly reduced and its only
determined by this method is 6.32 104 cm2 / V s. This mo-
contribution comes from grain-boundary diffusion.30 This
bility is smaller compared to other works.11 The poor elec-
should explain the absence of NWs in Fig. 1a.
trical conduction can be related to the low mobility presented
Next, we investigate the electrical properties of CuO
by the NW. The carrier concentration density is obtained to
NWs via the fabrication of FETs in a backgate configuration.
be around 1016 cm3 n0 = VthCox / qAL.38 This value is in
First, the NWs were dispersed in p-type silicon 100 nm
accordance with the result obtained by Seebeck
oxide layer by gently scratching the CuO forest sample into
measurements.39 Thus, despite the relatively high carrier
silicon substrate. Then, two metal contacts Cr/Au 10/100
concentration, the electrical conduction of the CuO NW is
nm were deposited on an isolated NW using optical lithog-
poor, limiting a wider application of this material. Further
raphy and thermal evaporation techniques. The SEM image
development on device fabrication e.g., use of different
of a fabricated device is shown in the inset of Fig. 7. The
metal contacts and growth process e.g., for doping needs
channel length between the electrodes is 15 m and its di-
to be performed to improve this behavior.
ameter is 250 nm. The calculated conductivity of an indi-
vidual CuO NW with no applied gate voltage Vg is 2.5
104 S / cm. This value differs from the CuO bulk 5.56
103 S / cm.35 We presented a systematic study on the growth of CuO
The source-drain current-voltage characteristics at differ- NWs by thermal oxidation. We propose that CuO NW
ent gates voltages are presented in Fig. 7a, where an in- growth occurs via grain-boundary diffusion of Cu ions
crease in the conductivity for negative gate voltages is ob- through the Cu2O layer of the oxygen ions through the top
served. Figure 7b depicts the I versus Vg voltages curve for CuO layer. The electrical properties of an isolated CuO NW
Vds fixed at 5 V. Its Ion / Ioff ratio is 15.5. These results dem- were determined by using a FET configuration. Intrinsic
onstrate that the CuO NWs have a p-type behavior. Little is p-type behavior and weak field effect response were ob-
known about the electrical properties of CuO NWs. For in- served. Such behavior can be attributed to low mobility,
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034303-5 Gonalves et al. J. Appl. Phys. 106, 034303 2009

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