620
P. Han et al. / Journal of Alloys and Compounds 664 (2016) 619e625
template assisted radio frequency magnetron sputtering, and the
electrodes of Ag were made by vacuum deposition. The preparation
sheets. The first anodization of Al sheet in 0.3 M H
was conducted for 12 h at 5 C. The anodized Al sheet was
2
C
2
O
4
solution
ꢀ
process is shown in Fig. 1. In addition, Ag/[MoSe
ture device displays an excellent photo-controlled bipolar resistive
switching behaviors, indicating the MoSe /TiO composite holds
2
/TiO
2
]/FTO struc-
completely removed in an aqueous acid mixture of H
3
PO
4
and CrO
3
ꢀ
(6 wt% and 1.8 wt%) at 60 C for 12 h. The second anodization was
ꢀ
2
2
carried out for 3 min at 5 C. The etching process in HgCl
2
at room
promise for practical applications of photo-controlled RRAM
devices.
temperature detached the alumina layer from the Al sheet. In
sequence, the barrier layer was removed by the pore widening
ꢀ
process with 5 wt% H
3
PO
4
at 30 C for 20 min. Finally, we obtained
2
. Experimental procedure
500 nm-thick AAO membranes that provided excellent contacts
with substrates.
2
.1. Preparation of MoSe and TiO
2
2
powder
MoSe
AAO nano-template by radio frequency magnetron sputtering
method. The MoSe nano-islands were deposited at room tem-
perature and the power of the radio frequency was set at 80 W. The
2
nano-islands were fabricated on FTO substrates through
In this work, MoSe
2
powder was synthesized by a hydrothermal
MoO $2H O) and sele-
2
method. Analytical sodium molybdate (Na
nium (Se) of analytical grade were used as precursor reagents
without any further purification. A stoichiometric amount of
Na
autoclave with a 50 ml capacity with stirring until completely
dissolved. Then an appropriate amount of hydrazine hydrate
2
4
2
ꢁ
1
deposition rate of MoSe
pressure for the deposition was 5.0 ꢂ 10 Pa and the Ar working
chamber pressure was 1.0 Pa. After MoSe deposition, extended
arrays of MoSe nano-islands were obtained by mechanically lifting
off the AAO mask. Then TiO film with the thickness of ~200 nm was
deposited on interspace of MoSe nano-islands at
2
was 0.02 nm s . The typical base chamber
ꢁ
5
2
MoO
4
$2H
2
O and Se powder was put into a stainless steel
2
2
2
(
N
H
2 4
2
$H O) was added into the tank under stirring. Distilled water
2
2
was added to fill the autoclave up to 80% of the total volume under
vigorous stirring for 30 min, and then the pH value was adjusted to
about 12 with the addition of solid NaOH. The autoclave was sealed
roomtemperature. Finally, the electrodes with the area of ~1 mm
and the thickness of ~200 nm were deposited on the same side for
the electric measurement by vacuum deposition.
ꢀ
and maintained at 180 C for 48 h, and then cooled to room tem-
perature naturally. A black precipitate was collected. After being
2.3. Material characteristics
washed with absolute ethanol and distilled water, the final product
ꢀ
was dried in a vacuum box at 60 C for overnight. Finally, we made a
Microstructure of MoSe
X-ray diffraction (XRD, Shimadzu XRD-7000 X-ray diffractometer)
with Cu K radiation. Surface morphology and energy dispersive X-
ray spectroscopy (EDX) spectra of MoSe /TiO compound grown on
FTO substrate was characterized using scanning electron micro-
scopy (SEM, JSM-6510). The microstructure characterization of the
2 2
/TiO compound was characterized by
target of magnetron sputtering using as-prepared MoSe
The TiO powder was prepared using the solegel method. TiO
powder was synthesized using titanium(IV) isopropoxide (TIP)
Aldrich Chemical, SigmaeAldrich Corporation, St. Louis, MO, USA),
nitric acid, ethyl alcohol, and distilled water. The TIP was mixed
with ethanol, and distilled water was added drop by drop under
vigorous stirring for 1 h. This solution was then peptized using
2
powders.
2
2
a
2
2
(
2 2
MoSe /TiO compound was tested by transmission electron mi-
croscopy (JEM-2100) at an acceleration voltage of 200 kV. The
chemical state was analyzed by X-ray photoelectron spectroscopy
(XPSESCALAB250).
ꢀ
nitric acid and heated under reflux at 80 C for 8 h. After this period,
a TiO
powder. The TiO
2
sol was prepared. The prepared sol was dried to yield a TiO
2
ꢀ
2
particles were annealed in air at 450 C for 1 h
using a programmable furnace to obtain the desired TiO
ometry and crystallinity. Similarly, we made a target of magnetron
sputtering using as-prepared TiO powders.
2
stoichi-
2.4. Device characteristics
2
In the test of resistive switching characteristics, Ag and FTO is
the top electrode and bottom electrode respectively. All the electric
measurements were measured using the electrochemical work-
station CHI-660D at room temperature. An ordinary filament lamp
with various power densities was used as light source. The spec-
trum of the light is shown in Fig. 2, which shows two peaks at
2 2
2.2. Preparation of Ag/[MoSe /TiO ]/FTO structure device
Anodic aluminum oxide (AAO) membranes with ~200 nm pore
size were fabricated by a two-step anodization of electropolished Al
Fig. 1. Schematics fabrication of Ag/[MoSe
2 2 2
/TiO ]/FTO structure device with MoSe
nano-island array inserted into TiO matrix grown on FTO substrate.
2
Fig. 2. The light spectra used as the light source in our experiment process.