Solar Energy Materials & Solar Cells 94 (2010) 2181–2186

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Solar Energy Materials & Solar Cells

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

Preparation and characterization of sol–gel Al-doped ZnO thin films and ZnO
nanowire arrays grown on Al-doped ZnO seed layer by hydrothermal method
Jin Zhang, Wenxiu Que n
Electronic Materials Research Laboratory, School of Electronic and Information Engineering, Xi’an, Jiaotong University, Xi’an 710049, Shaanxi, People’s Republic of China

a r t i c l e in fo abstract

Article history: Al-doped ZnO (AZO) nanocrystalline thin films are prepared by a sol–gel technique. Effects of the
Received 10 May 2010 Al-doped concentration on microstructural, electrical and optical properties of the AZO thin films are
Accepted 6 July 2010 studied and discussed. Results indicate that the AZO crystalline thin film with a highly preferred c-axis
Available online 19 August 2010
orientation perpendicular to the substrate is grown, and the AZO thin film with a small crystal grain size
Keywords: of 30–40 nm, high transmittance of above 90% in visible region, and low resistivity of 1.9  10  2 O cm
Zinc oxide can be obtained when the Al-doped concentration is up to 1 at%. Furthermore, ZnO nanowire (ZnO NW)
Nanowires arrays with a large surface area are grown on the sol–gel derived AZO thin film, which acts as a seed
Seed layer layer, by using a hydrothermal method. Optical properties of the grown ZnO NW arrays reveal that a
Sol–gel technique
high transmittance in visible region can be obtained, and only a strong UV emission at about 380 nm is
Photoluminescence
observed in the room-temperature photoluminescence spectra, which implies that few crystal defects
exist inside the as-assembled ZnO NW arrays.
& 2010 Elsevier B.V. All rights reserved.

1. Introduction
One-dimensional ZnO semiconductor nanostructures, such as
nanowires (NWs), nanospheres and nanoribbons, have attracted
increasing attention in recent years due to various applications
arising from their unique properties [1]. In particular, vertical ZnO
nanowire (ZnO NW) arrays are regarded as a promising candidate
for nanodevice assembly and applications in blue–UV light
emitters [2] and photodetectors [3], field emission devices [4]
and dye-sensitized solar cells [5]. Therefore, various methods
including thermal evaporation, solution method and epitaxy
technique have been employed to prepare the ZnO NW arrays
[6–8]. Although sapphire is the most frequently used substrate for
the growth of the ZnO NW arrays, it is not the best option to
prepare the ZnO NW devices because it is insulating and
expensive. The use of a lattice-matched and conducting buffer
layer may circumvent these problems [9–11]. Therefore, the ZnO
NW arrays grown on the doped ZnO seed layer are extensively
studied. For example, the Al-, Ga- and In-doped ZnO thin films
with high c-axis orientated crystalline structure along (0 0 2)
plane are extensively reported for practical applications including
transparent conducting electrode materials for various electronic
devices such as solar cells, electroluminescence displays, etc.
[12–16]. Among these doped ZnO thin films, Al-doped ZnO (AZO)
thin films are attractive owing to their good conductivity, high
transparency and relatively low cost [17,18]. Moreover, they can
be prepared by a variety of thin film deposition techniques
including radio frequency magnetron sputtering [19], chemical
vapor deposition [20], pulsed-laser deposition [21], sol–gel
process, etc. [18,22–26]. Among them, the sol–gel process is
simple and easy, and can prepare the possibility of a small or
large-area coating at relatively low temperature and cost [17,27].
In recent years, the luminescent and electron field emission
properties of the ZnO NW arrays grown on AZO seed layers are
studied by many researchers [20,28], but they reported the
preparation of the AZO seed layers and the growth of the ZnO NW
arrays by a radio frequency magnetron sputtering and a vapor–
liquid–solid (VLS) method, respectively, which require expensive
equipments and high process temperature. In this paper, the AZO
thin films were prepared by the sol–gel process, and effects of the
Al-doped concentration on microstructural, electrical and optical
properties of the as-prepared AZO thin films were investigated. In
addition, the ZnO NW arrays grown on the as-prepared AZO seed
layer were grown using a hydrothermal method and the optical
and morphological properties of the grown ZnO NW arrays were
also characterized and evaluated.
2. Experimental study

The AZO thin films and the ZnO NW arrays grown on the AZO
n
Corresponding author. Tel.: +86 29 82668679; fax: +86 29 82668794. seed layer were prepared and grown by a sol–gel technique and a
E-mail address: wxque@mail.xjtu.edu.cn (W. Que). hydrothermal method, respectively. Zn(CH3COO)2  2H2O was first

0927-0248/$ - see front matter & 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.solmat.2010.07.009
2182 J. Zhang, W. Que / Solar Energy Materials & Solar Cells 94 (2010) 2181–2186
dissolved in a 2-methoxyethanol-monoethanolamine (MEA)-deio-
nized water solution at room temperature. The molar ratio of MEA
and deionized water to zinc acetate was kept at 1 and 0.5,
respectively, and the concentration of zinc acetate was 0.75 mol/L.
Then appropriate amounts of aluminum doping were achieved by
adding AlCl3  6 H2O to the precursor solution. In order to study an
effect of the Al-doped concentration on microstructural, electrical
and optical properties of the AZO thin films, three solutions with
doped concentration of Al/Zn¼0, 1 and 2 at%, respectively, were
used. Then these solutions were stirred at 60 1C for 30 min to yield
clear and homogeneous solutions. The AZO thin films were
deposited on common glass substrate by a multi-spin-coating
process at 3000 rpm for 20 s. After depositing one layer, the thin
film was preheated in air at 200 1C for 10 min and the thickness of
the one-layer thin film was about 50 nm. The thin film was finally
post-heated at 500 1C for 1 h in air using an electronic furnace [29].
Corresponding to the different Al-doped concentrations (0, 1 and
2 at%), the obtained thin films were labeled as Sample A, Sample B
and Sample C, respectively. Followed that the vertical ZnO NW
arrays were grown in a Teflon-lined stainless steel autoclave by
immersing the substrates deposited with AZO seed layer in mixed
aqueous solution, which includes Zn(NO3)2 (0.04 mol/L) and NaOH
(0.8 mol/L), at 80 1C for 1 h. Finally, the samples were washed with
deionized water and dried in the air at 80 1C [30].
The structural properties of the thin films were characterized
using a D/max-2400 X-ray diffraction spectrometer (Rigaku) with Cu
Ka radiation and operated at 40 kV and 100 mA from 201 to 701 in
2y, and the scanning speed was 151 min  1 at a step of 0.021. The
morphological properties of the thin films were observed by a JEOL
JSM-7000F field-emission scanning electron microscope (FE-SEM).
The UV–vis absorption spectra and transmittance spectra of the thin
films were characterized by a JASCO V-570 UV/VIS/NIR spectrometer
and the photoluminescence spectra of the thin films were measured
at room temperature by a Fluoromax-4 spectrometer. The sheet
resistance (R&) of the AZO thin films was measured by a four-point
probe and the thickness (d) of the thin film was determined by a
Fig. 1. SEM images of the AZO thin films: (a) Sample A, (b) Sample B and (c) Sample C.
surface profile measurement system; thus the resistivity of the
resultant AZO thin films was calculated based on r ¼R& d.
3. Results and discussion
3.1. Microstructural and electrical properties of the AZO thin films
Fig. 1 shows the SEM images of the AZO thin film samples. It
can be seen that the AZO thin films with a uniform crystal grain
and flat surface morphology can be obtained by the sol–gel
technique under present process conditions, but the crystal grain
size of the sample changes with the Al-doped concentration,
which starts to decrease with the doping of the Al and then
increase with a further increases in the Al-doped concentration.
For example, the crystal grain size of Sample B is smaller than that
of Sample A due to the doping of 1 at% Al, but the crystal grain size
of Sample C is much bigger than those of Samples A and B. In
addition, it is also noteworthy that some particles can be clearly
observed on the surface of the thin film Sample C as shown in
Fig. 1(c). We suspect that it is probably related to an excessive
doping of the Al (up to 2 at%), that is to say, the superfluous Al
atoms may form some kind of crystal defects and some of these
defects accumulate together at the grain boundaries leading to
the big particles as shown in Fig. 1(c).
XRD patterns of the samples with different Al-doped concen-
trations are shown in Fig. 2. It can be seen from Fig. 2 that besides
the (0 0 2) diffraction peak of ZnO can be clearly observed, no
other peaks are detected, indicating that the as-prepared thin film
samples have a good crystalline structure and textured with their
c-axis oriented perpendicular to the substrate. Especially, the
diffraction peak of Sample B in intensity is the highest in all
three samples. The inset of Fig. 2 shows the partial enlarged
XRD patterns of the samples with the 2y in a range between
301 and 401. It can be noted that two faint crystal orientation
peaks of (1 0 0) and (1 0 1) can also be observed for Sample A, and
 J. Zhang, W. Que / Solar Energy Materials & Solar Cells 94 (2010) 2181–2186
these diffraction peaks can be assigned to the wurtzite hexagonal-
shaped ZnO. However, it should be stressed that these crystal
orientation peaks are almost not observed for Sample B, but the
intensities of these diffraction peaks are significantly enhanced
for Sample C as compared with those of Sample A. These results
indicate that the doping of 1 at% Al into the ZnO thin film not only
enhances the crystalline orientation of the (0 0 2), but also
decreases the intensity of the other plane peaks, while the
doping of 2 at% Al, the crystalline property of the (0 0 2)
orientation is obviously deteriorated owing to an appearance of
the (1 0 0) and (1 0 1) peaks, which is probably ascribed to an
excessive doping of the Al. These results further confirm those
obtained by SEM. Based on the Scherer equation and Bragg’s
law [31], the crystal grain size and the lattice constant of the
samples are estimated from the peaks as shown in Fig. 2. Table 1
summarizes the measured and the calculated values obtained
from the XRD curves. In addition, the resistivity of the as-prepared
AZO thin films is also presented in Table 1. A shift in the
diffraction peak at (0 0 2) to a large angle is also detected in these
Al-doped thin films as compared with Sample A (ZnO thin film) as
shown in Table 1, which reflects the lattice distortion induced due
to the substitution of Al3 + for Zn2 + . The crystal grain size of the
samples, which is calculated by the Scherer equation, is coincided
with the results obtained by SEM. According to the Bragg law, the
lattice constants of the samples can be figured out. It can be found
that the value of the lattice constant ‘‘a’’ increases and the lattice
constant ‘‘c’’ decreases with an increase in the Al-doped
concentration.
According to the above discussion, a lattice distortion model of
the AZO thin film can be established as shown in Fig. 3. From the
Intensity (a.u.)
Intensity (a.u.)
30
Sample C
Sample B
Sample A
20 30 40 50
2 Theta / degree
Fig. 2. XRD patterns of the AZO thin films.
Table 1
Comparison of 2y, crystal grain size, lattice constant and resistivity of the AZO thin films doped with different Al concentrations.
Samples 2y
Sample A 34.3765
Sample B 34.4226
Sample C 34.4631
2183
results of the XRD analysis, the lattice structure of the undoped
ZnO (Sample A) belongs to wurtzite hexagonal-shaped ZnO with
space group P63mc (Joint Committee on Powder Diffraction
Standards (JCPDS) card files 36-1451). It can be seen from
Table 1 that the lattice constant ‘‘c’’ and the crystal grain size of
sample B are smaller than those of Sample A, indicating that Zn2 +
is substituted by Al3 + at the lattice point of ZnO crystal as shown
in Fig. 3. This is because the radius of Al3 + ( 0.05 nm) is smaller
than that of Zn2 + (0.074 nm), thus leading to a decrease in the
lattice constant ‘‘c’’ and the crystal grain size of Sample B.
Furthermore, Al3 + with a smaller radius has higher mobility and
more easily getting across the crystal boundary than Zn2 + in the
annealing process. So it is possible to make Sample B have a better
crystalline orientation at (0 0 2) in comparison with Sample A as
shown in Fig. 2. However, with further increase in the doping of Al
up to 2 at% (Sample C), it is noted that the lattice constant ‘‘c’’ of
Sample C decreases, but the lattice constant ‘‘a’’ and the crystal
grain size increase significantly. These are probably related to the
superfluous Al atoms that form some kind of neutral defects such
as interstitial Al atoms and some of them are oxidized to form
Al2O3, which leads to the appearance of the crystal growth
orientation along (1 0 0) and (1 0 1) planes as shown in Fig. 2,
and the crystal grain size of Sample C increases at horizontal
direction. It is also seen from Table 1 that the resistivity of
Sample B (1.9  10  2 O cm) is lower than that of Sample C
(2.25  10  2 O cm). A possible explanation is as follows: when a
small amount of Al is introduced into the ZnO thin film, Al is
ionized into Al3 + and followed to replace Zn2 + . Thus one free
electron is produced from one Zn2 + replacement. Therefore, the
electron concentration increases with the increase in Al
concentration at first up to 1 at%. However with further increase
in Al concentration, these superfluous Al atoms may form some
(101)
kind of neutral defects including interstitial Al atoms and Al2O3 as
(100)
discussed above. Obviously, these neutral defects neither
Sample C contribute to the free electrons nor decrease the mobility of the
electrons. Moreover, the resistivity of the AZO thin films is also
Sample B related to the crystal quality of the thin film as reported in
Ref. [25]. It can be noted that the higher the crystal orientation at
Sample A (0 0 2), the lower the resistivity of the AZO thin films, which is
probably due to the shorter electron path length in (0 0 2) plane
35 40 and the reduction in the scattering of the electrons at the grain
2 Theta / degree boundaries and the crystal defects. It should be mentioned that
the measured resistivity of the AZO thin films is relatively high as
compared to those of the AZO thin films reported in Refs. [17,25].
It is probably related to the smaller grain size, which is
responsible for electron scattering and thus yields relatively low
conductivity. This is to say, the AZO thin films as reported in
Ref. [17,25] were obtained at a higher annealing temperature and
under a nitrogen environment. Thus, it is possible that the grain
size of the AZO thin film will grow bigger and thus decreases
electron scattering at the grain boundaries. On the other hand, the
60 70 oxidization probability of Al3 + is decreased when the AZO thin
film is annealed under a nitrogen environment, which makes
most of Al3 + be kept down and yield electrons. These factors
result in a relative low resistivity together.
Crystal grain size (nm) Lattice constants Resistivity (  10  3 O cm)
a c
52.7 3.24 5.24 –
35.5 3.25 5.23 19
61.3 3.26 5.23 22.5
2184 J. Zhang, W. Que / Solar Energy Materials & Solar Cells 94 (2010) 2181–2186
Fig. 3. Lattice distortion model of the AZO thin films doped with different Al concentrations.
100
80
Trans (%)
60
40
20
0 0.0
350 400 450 500
Wavelength (nm)
Fig. 4. Transmittance and absorption spectra of the AZO thin films: (a) transmittance spectra and (b) absorption spectra.
3.2. Optical properties of the AZO thin films
Effects of the Al-doped concentration on the optical properties
of the ZnO thin films are also studied. The thickness of the
thin films is about 100 nm by a twice spin-coating process. The
transmittance spectra of the AZO thin films with various Al-doped
concentrations are plotted in Fig. 4(a). All of the thin films exhibit
a transmittance of higher than 90% in the visible region.
A fluctuation in the spectral shape should be ascribed to
interference phenomenon between the top and the bottom
surface of the film. Fig. 4(b) shows the absorption spectra of the
samples. It is found that the absorption peak of the AZO thin films
has a blue shift as compared to that of the ZnO thin film. In
general, the blue shift of the absorption peak for the AZO thin
films is associated with the increase in the electron concentration
blocking the low states of the conduction band, well known as the
Burstein–Moss effect [32,33]. Burstein pointed out that the
increased electrons will fill in the low states of the conduction
band in the AZO thin films, which compels the electrons of
valence band to transit to the high states of the conduction band
when the AZO thin films are excited. Corresponding to optical
absorption, the UV absorption peak shifts to a short wavelength.
Furthermore, when the electron concentration of the AZO thin
film tends to saturation, the blue shift of the UV absorption peak
will be gradually weakened, which can also be seen in Fig. 4(b).
These indicate that the electron concentration of the AZO thin film
tends to a saturation when the Al-doped concentration is up to
2 at%.
3.3. Microstructural properties of the ZnO NW arrays grown on the
AZO seed layers
Fig. 5 shows the SEM images of the ZnO NW arrays grown on
the thin film Samples A, B and C, respectively. Here, Samples A, B
and C are employed as the seed layer for the growth of the ZnO
2.0
Sample A
Sample B
Sample A
Sample B
Sample C
Sample C
1.5
Abs (a.u.)
1.0
0.5
550 600 350 375 400 425 450
Wavelength (nm)
NM arrays. It can be seen that vertically aligned ZnO NWs grown
on the seed layer have an acicular structure. The diameter of the
ZnO NWs grown on Sample B is smaller and the distance between
the ZnO NWs is bigger than those of Samples A and C. This is
because the diameter of the ZnO NWs and the distance between
the ZnO NWs are dependent on the crystal grain size and the
crystal interspaces of the seed layer, respectively, which can be
confirmed by the results of Fig. 1. In addition, the quantity of the
crystal grains within the unit area of Sample B is more than those
of Samples A and C as can be observed in Fig. 1, which leads to the
larger number of the ZnO NWs grown on Sample B than those on
Samples A and C as shown in Fig. 5. Fig. 6 shows the relationship
between the length of the ZnO NW arrays and the Al-doped
concentration of the seed layer. It can be observed that the ZnO
NWs grown on Sample B have the longest length of the three
samples, and the length of the ZnO NWs grown on Sample A is a
little longer than that on Sample C. These results are probably
related to the crystal grain size of the sample. This is to say, the
bigger the crystal grain size, the shorter the grown ZnO NWs as
shown in Figs. 1 and 5. It can be concluded based on above results
and discussion that the ZnO NW arrays grown on Sample B have a
larger surface area than those obtained from Samples A and C,
indicating the ZnO NW arrays grown on Sample B are more
suitable for the applications in dye-sensitized solar cells.
3.4. Optical properties of the ZnO NW arrays grown on the AZO seed
layers
Fig. 7 shows the transmittance spectra, which are normalized
by film thicknesses of the ZnO NW arrays grown on Samples A, B
and C. It can be seen from Fig. 7 that the normalized
transmittance of the three samples in visible region is above
40%, and the regular wave shape of the transmittance curves
suggests the thickness of the ZnO NW arrays is uniform, which
can also be observed in the insets of Fig. 5. Furthermore, the
 J. Zhang, W. Que / Solar Energy Materials & Solar Cells 94 (2010) 2181–2186 2185

Fig. 5. SEM images of the ZnO NW arrays grown on the AZO seed layer (a) on Sample A, (b) on Sample B and (c) on Sample C.

1.8 100
ZnO NWs grown on Sample A
ZnO NWs grown on Sample B
1.7 80 ZnO NWs grown on Sample C
Normalized Trans (%)

1.6
Length / µ m

60

1.5
40

1.4
20

1.3
0
0.0at.% 0.5at.% 1.0at.% 1.5at.% 2.0at.% 400 500 600 700 800
Doping concentration Wavelength (nm)

Fig. 6. Relationship between the length of the ZnO NW arrays and the Al-doped Fig. 7. Transmittance spectra of the ZnO NW arrays grown on Samples A, B and C.
concentration.

transmittance of the ZnO NW arrays grown on Sample C is the
highest of the three samples, and the transmittance of the ZnO
NW arrays grown on Sample A is higher than that grown on
Sample B. A reasonable explanation is that the transmittance is
related to the surface roughness and the verticality of the ZnO NW
arrays. Large surface roughness and poor verticality of the ZnO
NW arrays lead to high light scattering and decreases light
transmittance. It can be observed that the ZnO NW arrays grown
on Sample B have larger surface roughness and poorer verticality
than those grown on Samples A and C as shown in Fig. 5. In
addition, room temperature photoluminescence (PL) spectra
(excite at 365 nm, 1 nm slit width) of the grown ZnO NW arrays
are also measured and shown in Fig. 8. Results indicate that a
sharp and strong UV peak at 380 nm dominates the PL spectra,
which should be assigned to the intrinsic excitation of ZnO; the
inset shows the partial enlarged PL spectra from 390 to 420 nm,
and no other peaks are observed in the curves. Thus, it is
reasonable to predicate that few crystal defects exist in the ZnO
NW arrays grown on the sol–gel derived AZO seed layers.
4. Conclusions
The AZO thin films have been successfully prepared by the
sol–gel method. Effects of the Al-doped concentration on micro-
structural, electrical and optical properties of the AZO thin films
have been studied. Results indicate that the as-prepared AZO thin
films have a wurtzite c-axis preferred orientation perpendicular to
2186 J. Zhang, W. Que / Solar Energy Materials & Solar Cells 94 (2010) 2181–2186
2.0x106
Intensity (a.u.)
1.5x106
Intensity (a.u.)
1.0x106
390 400 410
Wavelength (nm)
ZnO NWs grown on Sample A
5.0x105
ZnO NWs grown on Sample B
ZnO NWs grown on Sample C
0.0
380 390 400 410 420 430 440
Wavelength (nm)
Fig. 8. Normalized PL spectra of the ZnO NW arrays grown on Samples A, B and C.
the glass substrate, and the AZO thin film with small crystal grain
size, high transmittance and low resistivity can be obtained when
the Al-doped concentration is 1 at%. The ZnO NW arrays grown on
the sol–gel derived AZO seed layer, which has a high transmit-
tance in visible region, strong PL emission and few crystal defects,
have been obtained by the self-assemble process in the mixed
aqueous solution of Zn(NO3)2 and NaOH. Especially, when the
sample doped with Al concentration of 1 at% is used as the seed
layer, the grown ZnO NW arrays have a larger surface area, which
are suitable for the applications in the dye-sensitized solar cells,
luminescent and electron field emission devices.
Acknowledgments
This work was supported by the Ministry of Science
and Technology of China through 863-project under Grant
2009AA03Z218, the Major Program of the National Natural
Science Foundation of China under Grant no. 90923012, and Xi’an
Applied Materials Innovation Fund (XA-AM-200805).
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