Chemical Engineering Journal 170 (2011) 326332

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Chemical Engineering Journal

journal homepage: www.elsevier.com/locate/cej

Simply heating to remove the sacricial core TeO2 nanowires and to generate
tubular nanostructures of metal oxides
Hyoun Woo Kim a, , Han Gil Na b , Ju Chan Yang b
a
b

Division of Materials Science and Engineering, Hanyang University, 17 Haengdang Dong, Seongdong Gu, Seoul 133-791, Republic of Korea
Division of Materials Science and Engineering, Inha University, Incheon 402-751, Republic of Korea

a r t i c l e

i n f o

Article history:
Received 21 October 2010
Received in revised form 2 March 2011
Accepted 16 March 2011
Keywords:
Tellurium oxide
Nanostructures
Photoluminescence

a b s t r a c t
This paper reports a novel method for fabricating nanotubes, in which the nanowire-templates were
removed by simple heating in air. The morphology and structure of the composite nanowires were
controlled by varying the heating temperature. High-temperature heating was found to be effective
in removing the core TeO2 nanowires. The photoluminescence study indicated that the emission of the
core-shell nanowires originated mainly from the ZnO shell. The increased visible emission with increasing heating temperature was attributed to the increase in the number of structural defects in the ZnO
shell. The visible emission band was blue-shifted with increasing annealing temperature.
2011 Elsevier B.V. All rights reserved.

1. Introduction
Since the discovery of carbon nanotubes in 1991 [1], onedimensional (1D) nanostructured materials, including nanorods,
nanowires and nanotubes, have received considerable attention on
account of their remarkable physical properties and potential applications. Among the 1D structures, tubular or hollow nanostructures
have attracted particular interest for their special technological
applications due to not only the superior optical, electrical, thermal and mechanical properties, but also to their high efciently
and activity caused by their high porosity and large surface area
[2].
Many researchers have prepared inorganic nanotubes through a
variety of approaches, including plasma discharge [3], the rolling up
of thin lms [4], thermal evaporation [5,6], hydrothermal process
[7], sono-electrochemical methods [8], anodization [9,10], and catalyzed transport reaction [11]. Despite their scientic signicance
and potential applications, the in situ fabrication of nanotubes
has some shortcomings, in which precise control of the nanotube dimensions is limited. Accordingly, a casting method has
been illuminated, in which nanostructures with hollow interiors are commonly prepared by coating the surfaces of templates
with thin layers of the desired materials, followed by selective
removal of the templates through wet chemical etching [12,13]
or calcination [12,14,15]. However, wet chemical methods have
several disadvantages, including incomplete removal of the template, difculty in achieving a small enough diameter, and possible

Corresponding author. Tel.: +82 10 8428 0883.

E-mail address: hyounwoo@hanyang.ac.kr (H.W. Kim).
1385-8947/$ see front matter 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.cej.2011.03.066

environmental pollution. A range of calcination methods have been

implemented. Caruso et al. employed polystyrene latex particles as
templates, which were removed by exposure to tetrahydrofuran
[12]. Ji et al. used iced lipid nanotubes as templates, in which subsequent solgel process/calcination resulted in the transition metal
oxide nanotubes [15]. Goldberger et al. removed the ZnO nanowire
templates in NH3 or H2 ambient [16]. These methods require a complicated process with a precisely controlled scheme or an expensive
gas.
This communication reports the fabrication of metal oxide
nanotubes using a simple heating method. Compared to the
conventional calcination method, this technique provides a largerprocess-window, low-cost, clean and simpler process. In this
method, TeO2 nanowires were used as a sacricial template, which
can be removed easily by a simple heating technique (Fig. 1). To our
knowledge, this is the rst report of the use of TeO2 nanowires as
a sacricial template for the formation of nanotubular structures.
Ultimately, hollow ZnO nanotubes were obtained. Zinc oxide (ZnO)
is a promising material for applications as transparent electrodes
[17], gas sensors [18], acousto-optical devices [19], nanolasers
[20], piezoelectric devices [21] and short-wavelength optoelectronic devices owing its wide direct band-gap of 3.37 eV and a
large exciton binding energy of 60 meV. ZnO is also a biosafe and
biocompatible material that can be used directly for biomedical
applications without a coating [22].
In particular, ZnO nanotubes with a hollow structure will have a
variety of potential applications. The large thickness ratio of the
wall to the diameter suggests good eld emission performance
similar to the large aspect ratio of carbon nanotubes [23]. A large
surface areavolume ratio in ZnO tubular structures would provide an effective way of optimizing the performance of a range of

H.W. Kim et al. / Chemical Engineering Journal 170 (2011) 326332

327

Atomic layer deposition (ALD) of the ZnO shell layers on the core
TeO2 nanowires was carried out using diethylzinc (DEZn) and H2 O
as the Zn and O precursors, respectively (Fig. 1). The vaporization
temperature of DEZn and H2 O was set to 35 and 18 C, respectively
[32]. Ar carrier gas with ow rates of 100 sccm and 0 sccm was used
to deliver the DEZn and H2 O to the chamber, respectively. Ar gas
with a ow rate of 400 sccm was used for the line and chamber
purge. The DEZn injection time was 5 s, which was divided into 1 s
for sourcing without the carrier gas and 4 s for delivery with an Ar
gas ow rate of 100 sccm. The H2 O injection time was 5 s under a
variety of power conditions of remote VHF ICP (27.12 MHz, 200 W).
A sufcient time of 15 s was used to purge the sources so as to
prevent intermixing of the precursor and reactant. The number of
ALD cycles was set to 100. The substrate temperature was 200 C.
Subsequently, the core-shell nanowires were thermally annealed
in air ambient at temperatures ranging from 400 to 800 C (Fig. 1).
The pressure was maintained at less than 2 Torr by using the rotary
pump.
2.2. Characterization
Scanning electron microscopy (SEM) images were obtained
using a Hitachi S-4200. For SEM observation, the samples were
coated with Au using a turbo sputter coater (Emitech K575X,
Emitech Ltd., Ashford, Kent, UK). Glancing angle (0.5 ) X-ray diffraction (XRD) was performed using a Philips Xpert MPD system with
CuK1 radiation. Transmission electron microscopy (TEM) and
energy-dispersive X-ray (EDX) spectroscopy were carried out using
a Philips CM 200 operating at 200 kV. The PL spectra were measured at room temperature on a SPEX-1403 photoluminescence
spectrometer using the 325 nm line from a HeCd laser (Kimon,
Japan).
3. Results and discussion

Fig. 1. Schematic outline of the process sequence for the generation of metal oxide
nanotubes.

devices including dye-synthesized photovoltaic cells [24], catalysts,

photocatalysts [25], gas sensors [26], hydrogen storage [27], light
emitting diodes [28,29], and biosensors [30].
2. Experimental details
2.1. Synthesis of core-shell nanowires and subsequent thermal
heating
Core TeO2 nanowires were prepared by heating the source Te
powders in a high-temperature vertical tube furnace in N2 ambient
at a ow rate of 2 standard liters per min (slm) (Fig. 1). A schematic
diagram of the experimental apparatus is reported elsewhere [31].
Te powder (99.9%-purity) was used as the source material and
placed at the lower holder in the center of the quartz tube. The
Si plate coated with a 3-nm Au layer was placed in the upper
holder, which acted as a substrate for collecting the growth products. The Au layer was sputtered by ion sputterer (Emitech, K757X).
The vertical distance between the powders and the substrate was
approximately 7 mm. The substrate was set to 400 C in a nitrogen
(N2 ) gas ow, in which the gas ow rate was 2 standard liter per
min (slm). After a typical 1 h deposition process, the substrate was
cooled and removed from the furnace.

Fig. 2a shows an SEM image of the TeO2 nanowires used as templates, indicating the large-scale production of the nanowires. The
XRD pattern of the TeO2 nanowires in Fig. 2b shows that almost
all peaks could be indexed to tetragonal tellurium oxide with lat which are consistent with
tice constants of a = 4.81 A and c = 7.61 A,
the standard literature values (JCPDS no. 42-1365). The enlarged
SEM image and low-magnication TEM image showed that the
nanowires had maintained their circular-rod-like and continuous
morphology despite the shell coating (Fig. 2c and d). On the other
hand, the TeO2 /ZnO core-shell nanowires exhibited XRD peaks
with respect to tetragonal TeO2 , orthorhombic TeO2 (JCPDS no.
09-0433) and hexagonal ZnO (JCPDS no. 36-1451) (Fig. 2e). Accordingly, the ZnO shell layer was comprised of a crystalline phase. XRD
(Fig. 2b and e) conrmed the conversion of a tetragonal TeO2 to an
orthorhombic TeO2 structure at approximately 200 C, which was
the substrate temperature during the ALD process. This is in contrast to previous reports in which an orthorhombic to tetragonal
phase transition in TeO2 thin lms occurred during thermal annealing [33]. S-1 (Supplementary materials) shows the lattice-resolved
TEM image and selected area electron diffraction (SAED) pattern of
the TeO2 /ZnO core-shell nanowires, conrming that the shell layer
was comprised of a hexagonal ZnO phase.
Subsequently, thermal annealing was carried out at 400, 600
and 800 C. Fig. 3 shows the changes in the structure and morphology of the TeO2 /ZnO core-shell nanowires after thermal annealing.
S-2 (Supplementary materials) presents the diameter distribution
of the samples annealed at 400, 600 and 800 C based on statistical analysis of the SEM images. The maxima of the diameter
distributions of the samples annealed at 400, 600 and 800 C were
130140 nm, 8090 nm, and 7080 nm, respectively. The mean

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Fig. 2. (a) SEM image and (b) XRD pattern of the as-synthesized TeO2 nanowires. (c) SEM image and (d) TEM image of a TeO2 /ZnO core-shell nanowire. (e) XRD pattern of
the TeO2 /ZnO core-shell nanowires.

diameter of the nanowires annealed at 400, 600 and 800 C, which

was calculated from the graph of the diameter distributions, was
131 nm, 96 nm and 85 nm samples, respectively. The nanowire
diameter decreased with increasing annealing temperature.
The XRD pattern of 400 C-annealed sample on the righthand-side of Fig. 3a revealed the presence of tetragonal TeO2 ,
orthorhombic TeO2 , rhombohedral TeO3 (JCPDS no. 85-0747), and
cubic Au (JCPDS no. 04-0784). Some TeO2 phase may have transformed to TeO3 by thermal annealing at 400 C. In addition, the XRD
patterns of the samples annealed at 600800 C showed no signs of
tellurium oxide-related peaks (Fig. 3b and c).
Fig. 4a shows a low magnication TEM image of the core-shell
nanowire annealed at 400 C. Fig. 4b shows the corresponding SAED
pattern, indicating that it is comprised of diffusion rings, which
are associated with hexagonal ZnO, orthorhombic TeO2 and rhombohedral TeO3 . The lattice-resolved TEM image shown in Fig. 4c
revealed the lattice planes of hexagonal ZnO and rhombohedral
TeO3 .
On the other hand, the 600 C-annealed nanowires (Fig. 4d)
exhibited a contrasted image with the core and shells as bright and
dark regions, respectively. The line concentration proles shown
in the upper-right inset showed that the relative amount of Te was
considerably smaller than Zn, indicating that the proportion of Te
was reduced signicantly by thermal annealing at 600 C. The SAED
pattern (Fig. 4e) and lattice-resolved TEM image (Fig. 4f) coincidentally indicated that the 600 C-annealed sample consisted mainly
of the hexagonal ZnO phase. In addition, the ring-like SAED pattern
revealed the samples to be polycrystalline.
Fig. 5a is a low-magnication TEM image of the core-shell
nanowires annealed at 800 C. The nanostrucure had a relatively
rough surface. In conjunction with S-2, it is believed that the nanostructure was silghtly contracted and deformed. Furthermore, some
voids were observed in the nanostructure. Fig. 5b is a corresponding line concentration prole that exhibits a valley-like prole

for Zn and O with a negligible amount of Te. Both SAED patterns

(Fig. 5c) and lattice-resolved TEM images (Fig. 5d) showed that the
nanostructure consisted mainly of a polycrystalline hexagonal ZnO
structure.
It is unclear why the core TeO2 nanowires could be removed
efciently by thermal heating. The vaporization of solid TeO2 can
be activated at higher temperatures. Since the contribution of all
other tellurium-bearing gas species, such as (TeO2 )2 , TeO, (TeO)2 ,
Te2 , to the total pressure was estimated to be <5% [34], it was
surmised that the vapor consisted mainly of monometric TeO2 (g)
species. Expression (1) shows the temperature dependence of the
TeO2 vapor pressure [35].
TeO2 (s) = TeO2 (g)
log p (atm) = 8.067

12, 000
T

(846 < T < 1006 K)

(1)

The vapor pressures of TeO2 at 400 and 600 C are 1.7 1010
and 2.1 106 atm, respectively, suggesting a drastic increase in
the TeO2 vapor pressure at higher temperatures. This indicates that
a variety of materials with an acceptably low vapor pressure can be
a candidate for sacricial templates.
Since the boiling temperature of TeO2 is 1245 C, we reveal that
the TeO2 nanowires have been evaporated at temperatures which
are considerably lower than their boiling temperature. We surmise
that this observation is due to the size effect, in which the evaporation temperature of nanocrystals is found to be size-dependent
and decreases with decreasing size, i.e. diameter of nanoparticles
and nanorods, or thickness of thin lms [36]. A TGA curve from
the bundles of TeO2 nanowires tested at 760 Torr indicates that
the evaporation occurred at about 816 C, which is considerably
lower than their boiling temperature (1245 C) (Supplementary
materials, S-3). By the way, in the present paper, the evaporation
of TeO2 nanowires seemed to start below 800 C. The heating of

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329

Fig. 3. SEM images and associated XRD patterns of the TeO2 /ZnO core-shell nanowires annealed at (a) 400, (b) 600, and (c) 800 C.

the TeO2 /ZnO core-shell nanowires was carried out at a pressure

of <2 Torr, with the rotary pump. On the contrary, the TGA experiments (S-3) were performed at a pressure of 760 Torr. Accordingly,
we expect that the actual TGA curve of the TeO2 /ZnO core-shell
nanowires in the present paper will shift to the left, in comparison to the curve of TeO2 nanowires tested at 760 Torr. Under the
lower ambient pressure, TeO2 is supposed to evaporate at a lower
temperature.
Fig. 6 shows the PL spectra of various samples measured at room
temperature. The PL spectrum of the uncoated TeO2 nanowires
corresponds to the band centered at approximately 2.7 eV in the
blue region (Supplementary materials, S-4). A similar blue band
has been observed with TeO2 crystals, which is probably excitonic
in nature [37]. In terms of Gaussian tting analysis, the PL spectrum of the ZnO-coated TeO2 nanowires was deconvoluted into two
emission bands peaked at approximately 2.3 eV (green) and 3.2 eV
(ultraviolet (UV)), respectively (S-4). This was attributed to the typical emission from ZnO, with no blue emission from TeO2 being
observed, presumably due to the covering effect. The UV emission

band peaking at 3.23.3 eV corresponds to near band edge (NBE)

emission, which is associated with the excitons in ZnO [38,39]. The
broad green (or visible) emission band is related to emission from
the deep trapping sites corresponding to defects, such as oxygen
vacancies in ZnO [3841].
Annealing at 400 C did not noticeably change the PL spectrum
of the as-synthesized sample. In terms of Gaussian tting analysis, the PL spectra of the ZnO-coated TeO2 nanowires annealed at
600800 C were deconvoluted into two emission bands at approximately 2.5 eV (green) and 3.2 eV (ultraviolet (UV)), respectively
(S-4). The peak position of visible emission for ZnO-coated TeO2
nanowires was blue-shifted to 2.5 eV after thermal annealing at
higher temperatures (600800 C). The visible emission was quite
broad, covering a wide range of energy/wavelengths. The emission
of the sample annealed at 400 C extended from approximately 1.7
(red) to 2.6 eV (blue). In addition, the visible emission of the samples annealed at 600800 C extended from approximately 2.0 (red)
to 2.9 eV (blue). The yellow and green luminescence bands were
associated mainly with VZn and OZn defects, respectively [42,43]. At

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Fig. 4. (a) Low-magnication TEM image, (b) SAED pattern, and (c) lattice-resolved TEM image of TeO2 /ZnO core-shell nanowires annealed at 400 C. (d) Low-magnication
TEM image (inset: EDX concentration prole along the line drawing across the diameter of the coated nanowire), (e) SAED pattern, and (f) lattice-resolved TEM image of
TeO2 /ZnO core-shell nanowires annealed at 600 C.

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331

Fig. 5. (a) Low-magnication TEM image, (b) EDX concentration prole along the line drawing across the diameter of a coated nanowire, (c) SAED pattern, and (d) latticeresolved TEM image of TeO2 /ZnO core-shell nanowires annealed at 800 C.

higher temperature, many oxygen atoms in air ambient enter the Zn

vacancy to generate OZn . With increasing annealing temperature,
more oxygen atoms form OZn resulting in a gradual decrease in the
concentration of VZn in the ZnO shell. Accordingly, at higher annealing temperatures, the yellow emission may shift to green emission,
contributing to the overall blue-shift in the visible emission band.
Fig. 7 presents the relative intensities of the visible and UV emission for various samples. Figs. 6 and 7 show that the intensity of
visible emission from the ZnO-coated TeO2 nanowires increases
with increasing annealing temperature, whereas that of UV emission is relatively unaffected by temperature. Accordingly, we reveal

Fig. 7. Relative intensities of visible and UV emissions for TeO2 /ZnO core-shell
nanowires.

that a larger number of structural defects in the ZnO shell has been
generated during the annealing process at higher temperatures.
4. Conclusions

Fig. 6. PL spectra of (a) TeO2 nanowires and (be) TeO2 /ZnO core-shell nanowires,
which were (b) as-fabricated, (c) 400 C-annealed, (d) 600 C-annealed, and (e)
800 C-annealed.

Tubular structures of ZnO were fabricated by heating ZnOcoated TeO2 nanowires. The ZnO-coated TeO2 nanowires were
produced by coating ZnO shell layers on core TeO2 nanowires
by ALD. XRD showed that the core-shell nanowires annealed at
600800 C were comprised only of a hexagonal ZnO phase. On the
other hand, those heated at 400 C revealed additional peaks for
tellurium oxides. TEM and EDX showed that the 800 C-annealed
sample had contracted and deformed into a hollow tubular struc-

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H.W. Kim et al. / Chemical Engineering Journal 170 (2011) 326332

ture. The room-temperature PL spectra of the ZnO-coated TeO2

nanowires revealed visible and UV emission due to the ZnO shell.
The intensity of visible emission increased with increasing annealing temperature, whereas that of UV emission was relatively
unaffected. This was attributed to an increase in the number of
structural defects in the ZnO shell by annealing at higher temperatures. The overall blue-shift of the visible emission band by
increasing the annealing temperature was attributed to the change
in VZn to OZn defects.
Acknowledgements
This research was supported by National Nuclear R&D Program through the National Research Foundation of Korea (NRF)
funded by the Ministry of Education, Science and Technology
(2010-0018699).
Appendix A. Supplementary data
Supplementary data associated with this article can be found, in
the online version, at doi:10.1016/j.cej.2011.03.066.
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