Reactive Sputtering of Plasmonic Pt/ZnO Films for Decomposition of Gas-Phase Methanol under Visible Light

Article abstract of DOI:10.1002/cplu.201402175

The preparation of ZnO films by a versatile and effective facing-target sputtering method under various sputtering pressures is described. The ZnO films are coated with an ultrathin (2 nm) Pt layer through dc diode sputtering to form hybrid Pt/ZnO photocatalytic films. Interestingly, the Pt/ZnO films show an efficient visible-light photoresponse for the decomposition of gas-phase methanol owing to the unique surface plasmon resonance of the Pt film.

Full text of DOI:10.1002/cplu.201402175

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DOI: 10.1002/cplu.201402175
Reactive Sputtering of Plasmonic Pt/ZnO Films for
Decomposition of Gas-Phase Methanol under Visible Light
[
a]
[a]
[a]
[a]
[a]
Hongjun Wu,* Yue Ma, Yang Wang, Yang Gao, Dandan Yuan, and
[b]
Zhonghai Zhang*
The preparation of ZnO films by a versatile and effective
facing-target sputtering method under various sputtering pres-
sures is described. The ZnO films are coated with an ultrathin
so on. Among these methods, noble metal coating is a promis-
ing approach because of the excellent chemical and photo-
chemical stability obtained, especially its unique surface plas-
[24–26]
(2 nm) Pt layer through dc diode sputtering to form hybrid Pt/
mon resonance.
However, the amount of noble metal
ZnO photocatalytic films. Interestingly, the Pt/ZnO films show
an efficient visible-light photoresponse for the decomposition
of gas-phase methanol owing to the unique surface plasmon
resonance of the Pt film.
used should be as low as possible in the coating process
owing to the scarcity and high cost of these materials.
[27]
[28]
Recently, some metal oxide films such as TiO , WO3, and
2
[29]
Fe O3 films have been prepared successfully through the re-
2
active sputtering technique,. In addition, ZnO films under dif-
ferent mixed gas ratios were also prepared, and their photoca-
talytic activities under UV light illumination were discussed in
Over the past few decades, ZnO has attracted considerable at-
tention as a promising photocatalyst for water and air purifica-
[30]
our previous paper.
In this study, the reactive sputtering
[
1,2]
tion.
ZnO is one of the most suitable materials for the pho-
technique is used to deposit ZnO films with two facing Zn
tocatalytic process under illumination with ultraviolet light; the
typical electron mobility in ZnO is 10–100 times higher than
metal targets at a fixed gas ratio of Ar/O =6:4 under various
2
sputtering pressures (Ps) of 0.1, 0.5, 1.0, and 3.0 Pa. The pre-
pared ZnO films are coated with an ultrathin Pt layer (thickness
2 nm) to enhance the photocatalytic activity and extend the
photoresponse region to visible light. Sputtering at room tem-
perature is a simple and scalable method that allows the cir-
cumvention of postannealing or liquid deposition procedures
that can induce corrosion of the ZnO, but offers good control
of the deposited material quantity, repartition uniformity, and
attachment.
that in TiO , which leads to a reduced electrical resistance and
2
[
3]
enhanced electron transfer efficiency. ZnO can be prepared
through several chemical and physical methods such as sol-gel
[
4,5]
[6]
methods,
ultrasonic spray pyrolysis, metal organic chemi-
[
7,8]
[9,10]
cal vapor deposition,
pulsed laser deposition,
and sput-
[
11–13]
tering methods.
Among them, reactive sputtering deposi-
tion has shown more advantages including control of the pre-
ferred crystalline orientation, growth at a relatively low temper-
ature, no need for post-calcination, good interfacial adhesion
to the substrate, and a high packing density of the grown
Gas-phase methanol is used as the target molecule for pho-
tocatalytic decomposition. Methanol is a common indoor air
pollutant, and is harmful to human health. In addition, metha-
nol is one of the simplest CꢀHꢀO molecules, and with the help
of Fourier-transform infrared (FTIR) spectroscopy, the photoca-
talytic mechanism of methanol decomposition can be analyzed
easily. Although the photocatalytic activities of ZnO films have
been studied extensively, to the best of our knowledge, there
has been no report on sputtering Pt/ZnO films for gas-phase
photocatalytic application under visible light illumination.
A schematic diagram of the reactive system is shown in
Figure 1. The two Zn metal targets facing each other were sep-
arated by a distance of 100 mm, and the substrates were
placed at a distance of 50 mm from the middle of a straight
line connecting the centers of the target planes. Zn rectangu-
lar plates (68 mm long, 48 mm wide, 3 mm thick, purity 99.9%)
and glass slides were used as targets and substrates, respec-
tively. After the sputtering chamber was evacuated to a back-
[
14,15]
film.
The major disadvantage of ZnO is its high bandgap of
.2 eV, excited by light in the UV region, which is only about
–5% of the solar spectrum reaching the earth’s surface. For
3
3
the effective and practical utilization of solar light, it is necessa-
ry to modify the ZnO material to obtain a visible-light photo-
response. Many methods have been used to extend its photo-
[
16–19]
response region, such as nonmetal species doping,
dye
and
[
20,21]
[22,23]
sensitization,
the use of hybrid semiconductors,
[
a] Prof. H. Wu, Y. Ma, Y. Wang, Y. Gao, D. Yuan
Provincial Key Laboratory of Oil & Gas Chemical Technology
College of Chemistry & Chemical Engineering
Northeast Petroleum University, Daqing 163318 (P. R. China)
Fax: (+86)459 6619963
E-mail: hjwu@nepu.edu.cn
[b] Prof. Z. Zhang
ꢀ
4
Department of Chemistry
ground pressure below 2ꢀ10 Pa, the ZnO films were depos-
ited reactively at a dc input power of 100 W. A series of sam-
ples was prepared at various Ps values from 0.1 to 3.0 Pa. The
ultrathin Pt layer of about 2 nm in thickness was coated on the
surface of the as-deposited ZnO films with an auto fine coater
East China Normal University
Dongchuan Road 500, Shanghai 200241 (P. R. China)
Fax: (+86)21 54345359
E-mail: zhzhang@chem.ecnu.edu.cn
Supporting information for this article is available on the WWW under
http://dx.doi.org/10.1002/cplu.201402175.
ꢁ
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ferent Ps values; the (002) diffraction peak is the dominant ori-
entation, and the crystalline intensity depends on Ps. With in-
creasing Ps, both peaks of (002) and (103) increase in intensity
and sharpness. The crystal structure of the (002) direction may
2
+
2ꢀ
be explained from the reaction of Zn and O , and the con-
2
+
2ꢀ
centrations of Zn and O are much higher if high-energy
2
ꢀ
electrons produce O ions through inelastic collisions, as re-
[32]
ported by Shibata. The formation of the crystal structure of
the (103) pattern is the result of the reaction between neutral
Zn and neutral O . The increase in the (002) peak intensity at
2
high Ps may be explained by the fact that with increasing Ar
partial pressure, the ionization of Zn increases and an excess
of neutral O is produced. This contributes to the increase in
2
intensity of both the (002) and (103) patterns. For assessment
of the quality of the thin films, the full-width at half-maximum
(
FWHM) values of the (002) peak and the crystallite dimension
were estimated according to the Debye–Scherrer equation, as
Figure 1. Schematic diagram of the reactive sputtering system.
given in Equation (1), in which D is the crystallite dimension,
l is the wavelength of X-ray radiation (CuK =0.15406 nm), q is
a
[33]
(
(
FESEM, Zeiss SigmaHV) by controlling the sputtering current
20 mA) and time (30 s).
the diffraction angle, and b is the FWHM.
D ¼ 0:94l=bcosq
ð1Þ
The film thicknesses of all the ZnO films were measured
with a DEKTAK surface profiler with different sputtering times
Figure S1 in the Supporting Information). The sputtering time
The relationship between Ps and crystallite dimension is
shown in the inset of Figure 2. As Ps increases from 0.1 to
(
and film thickness showed a linear relation, and the sputtering
rates were calculated for different Ps values (inset in Figure S1).
For comparison of the photocatalytic activities of the ZnO
films, they were prepared with the same thickness of 500 nm
at different Ps by controlling the sputtering time.
3
.0 Pa, the grain size increases. According to Equation (1), the
mean crystallite sizes vertical to the c axis are 14.01, 15.51,
6.09, and 20.68 nm at Ps values of 0.1, 0.5, 1.0, and 3.0 Pa, re-
1
spectively.
The crystal structures of the ZnO films were characterized by
grazing incidence X-ray diffraction (GIXRD) using an X-ray dif-
fractometer (Shimadzu XRD-6000) with a CuKa source in the
range 2q=20–908. Figure 2 shows the GIXRD patterns of ZnO
films deposited at different Ps. It can be seen that all the peaks
of the samples are in good agreement with the wurtzite struc-
The surface morphologies of ZnO films were analyzed by
field-emission scanning electron microscopy (FE-SEM) (JEOL,
FE-SEM 6700). The FE-SEM images presented in Figure 3 allow
[
31]
ture (JCPDS card, No. 36-1451). No characteristic peaks are
observed for any other impurities. The clear and sharp diffrac-
tion peaks also reveal that the deposited ZnO film is of high
quality. The preferred orientation does not change with the dif-
Figure 3. FE-SEM images of ZnO film prepared at different sputtering pres-
sures: A) 0.1 Pa, inset is the EDS of Pt/ZnO films, B) 0.5, C) 1.0, and D) 3.0 Pa
at low magnification, and a) 0.1, b) 0.5, c) 1.0, and d) 3.0 Pa at high magnifi-
cation.
the investigation of the effect of different Ps values on the
ZnO film surface. The FE-SEM images of the ZnO film prepared
at higher Ps show relatively larger individual grain sizes, and
the grain boundaries are clearer. With increasing Ps, more Ar
2
+
atoms attack the Zn metal target, and more Zn is excited,
2
+
whereas the mobility of Zn is slow at high pressures, causing
2
+
the slow reaction rate of the Zn and O atom, as shown by
the sputtering rate results in Figure S1. The slow reaction rate
2
+
and high Zn concentration cause the larger grain size. The
Pt/ZnO films show the same surface morphology as the ZnO
Figure 2. GIXRD patterns of ZnO films prepared at different sputtering pres-
sures. The inset shows the Debye–Scherrer analysis of ZnO crystal size.
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films because of the ultrathin thickness of the Pt layer. This
result is in good agreement with the analysis of the XRD char-
acteristics. In addition, the ultrathin Pt layer cannot be identi-
fied in the SEM images, but the corresponding energy disper-
sive spectrum (EDS, equipped with FESEM) proves its existence
According to Equation (2), the bandgap of the as-deposited
ZnO film is measured to be about 3.26 eV. All the ZnO samples
exhibit nearly the same optical edge, which indicates that the
variation in pressure had no significant effect on the optical
absorption edge. After Pt deposition, the Pt/ZnO films showed
a weak redshift of the optical edge, which agreed well with
previous reports that the plasmonic absorption of Pt lies in the
(Figure S2).
The optical properties of ZnO films and Pt/ZnO were mea-
[35,36]
sured with a Jasco V-550 spectrophotometer at room tempera-
ture in the wavelength range 300–900 nm. Figure 4 shows the
UV and blue wavelength region.
The photocatalytic decomposition of methanol (5 mL) in the
gas phase was evaluated by FTIR spectroscopy (JASCO 480
plus), by measuring the concentration decay in a cylindrical
cell (9.8 cm length and 3.6 cm width) containing the Pt/ZnO
samples of surface area 2.5ꢀ6.7 cm. A schematic diagram of
the photocatalytic gas cell is shown in Figure 5. The photocata-
Figure 5. Schematic diagram of the photocatalytic reactor.
lytic degradation of methanol is performed under irradiation
ꢀ
2
by an artificial sunlight simulator of 100 mWcm (model: SET-
40F, Seric LTD, Japan) with filter cutting from 420 to 780 nm
1
for visible light, and from 350 to 780 nm for UV+visible light.
Figure 6a shows the FTIR spectra of methanol decomposi-
tion as a function of irradiation time under visible light illumi-
nation. The undissociated methanol shows bands at 1015,
ꢀ
1
1
055, 2855, 2972, and 3680 cm at an irradiation time of zero.
ꢀ
1
The double bands at 1015 and 1055 cm are attributed to the
CꢀO and CꢀH stretching regions. The bands at 2855 and
Figure 4. a) Optical transmittance spectra of the ZnO and Pt/ZnO films at dif-
ꢀ1
2
972 cm correspond to the symmetric and asymmetric vibra-
ferent sputtering pressures; b) the bandgap determination of ZnO and Pt/
[
37,38]
tions of the methoxy group (CH OC), respectively.
The band
2
3
ZnO from curves of (ahn) versus hn.
ꢀ
1
observed at 3680 cm could be assigned to the OH stretching
mode of intermediate species probably present at room tem-
[39]
variation in transmittance of the ZnO and Pt/ZnO films pre-
pared at different Ps values of 0.1–3.0 Pa. The Pt/ZnO films
show a much lower transmittance at wavelengths of 400–
perature. On the basis of the experimental data, we illustrate
the variation in the peak heights of bands in Figure 6b. With
the increasing irradiation time, the bands at 1015, 1045, 2860,
ꢀ
1
900 nm than the ZnO films for all the different Ps values, which
2950, and 3685 cm start to decrease in intensity and new
peaks appear at 669, 933, 1169, 1456, 1645, 1760, and
indicates that the ultrathin Pt film enhances the visible-light
absorbance of the ZnO films. This result implies the possibility
of visible-light photocatalytic applications of Pt/ZnO films.
The optical absorption edge of the ZnO and Pt/ZnO films is
around 380 nm. For a direct transition, the optical bandgap
ꢀ
1
ꢀ1
2350 cm . The bands at 1169 and 1760 cm can be assigned
to the CꢀO and C=O stretching vibration modes, respective-
[40,41]
ꢀ1
ly.
The band at 1456 and 1645 cm can be assigned to
the out-of-plane asymmetric bending of CꢀH and isolated C=
C, respectively. Notably, the absorption bands at 1015,
[42,43]
(
Eg) of the ZnO film is determined using Equation (2) in which
ꢀ
1
a is the absorption coefficient and hn is the energy of the inci-
1055, and 3680 cm almost disappear after 3 h of irradiation,
[
34]
ꢀ1
dent photon.
whereas the bands at 2855 and 2972 cm are still present
with decreasing intensities. Gaseous CO is a linear molecule
2
1=2
ꢀ1
aðhnÞ / AðhnꢀEgÞ
ð2Þ
with two infrared-active absorption bands at 2350 cm (anti-
ꢀ
1
symmetric stretching mode) and 669 cm
(bending
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Figure 6. a) Decomposition of methanol on Pt/ZnO films as a function of irradiation time; ZnO films were deposited at 0.1 Pa with a fixed gas ratio of 6:4
ꢀ
1
under illumination with visible light. b) Variation in peak heights of different bands. c) Variation in peak height at 2350 cm corresponding to the normal vi-
bration of CO molecules derived from the FTIR transmittance spectra with irradiation time on Pt/ZnO film at different sputtering pressures under illumination
2
of visible light and UV+visible light. d) Histogram of rate constants (k) on Pt/ZnO films: A) 0.1 Pa, UV+vis light, B) 0.1 Pa, visible light, C) 0.5 Pa, UV+vis light,
D) 0.5 Pa, visible light, E) 1.0 Pa, UV+vis light, F) 1.0 Pa, visible light, G) 3.0 Pa, UV+vis light, H) 3.0 Pa, visible light.
[
44,45]
mode).
Hence, one can conclude that the primary two
size increases with increasing Ps, which results in a lower
active surface area, and prohibits the surface from forming
better connections with the Pt thin layer. At high Ps, the high
ꢀ
1
peaks centered at 2350 and 669 cm imply the formation of
CO gas upon methanol decomposition.
2
2
+
Figure 6c shows the CO2 transmittance peak height
concentration of Zn reacts with O atoms, which increases
the oxygen vacancies in the formed ZnO film. Similar results
have been reported regarding a decrease in photocatalytic ac-
ꢀ
1
(
2350 cm ) of Pt/ZnO films deposited at different Ps under illu-
mination of visible light and UV+vis light. It is observed that
the variation in the photocatalytic activities of the Pt/ZnO films
depends on the Ps value. With increasing Ps, the photocatalytic
[
46,47]
tivity with an increasing number of oxygen vacancies.
The photocatalytic decomposition mechanism under visible
light is also discussed in this paper. The presence of the ultra-
thin Pt layer enhances the absorbance of the ZnO film in the
visible region and effectively transfers the photogenerated
electrons and separates the photoelectrons and photoholes,
which restrain the recombination of photogenerated charge
carriers, and therefore improve the photocatalytic activity of
the as-deposited ZnO films. As indicated in Figure 6a,b, the ox-
activity of the Pt/TiO films decreases under both visible light
2
and UV+vis light. The experimental data in Figure 6c are
found to fit approximately a pseudo-first-order kinetic model
by the linear transforms f(t)=f [1ꢀexp(ꢀkt)] (f is the peak
inf
height, f is the peak height at infinite time, and k is the rate
inf
constant). The values of the rate constant, k, and regression co-
efficient are plotted in Figure 6d. The pure ZnO did not show
any decomposition of methanol under visible light (Figure S3).
The visible light contribution in the photocatalytic processes
on the Pt/ZnO is over 50%, which can be ascribed to the sur-
face plasmon resonance effect of Pt on the ZnO films.
idative pathway of CH OH may undergo the processes shown
3
in Equations (3) to (10) on Pt/ZnO films.
eꢀ þ Pt ! Ptꢀ
ð3Þ
ð4Þ
ð5Þ
As Ps decreases, the photocatalytic activity of the Pt/ZnO
film is enhanced. The improvement in the photocatalytic activi-
ties of Pt/ZnO films deposited at low pressures may be caused
by the different surface morphology and crystal structure, as
indicated by the results of SEM and XRD analysis. The grain
ꢀ
ꢀ
2
Pt þ O ! CO
2
þ
ꢀ
ZnO þ hn ! h þ e
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ꢀ
ꢀ
2
e þ O ! CO
ð6Þ
ð7Þ
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9
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[
[
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[
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Keywords: heterogeneous catalysis · oxides · photocatalysis ·
platinum · semiconductors
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3
Received: June 11, 2014
2
Published online on && &&, 0000
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2014 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
ChemPlusChem 0000, 00, 1 – 5
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5
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These are not the final page numbers!

COMMUNICATIONS
H. Wu,* Y. Ma, Y. Wang, Y. Gao, D. Yuan,
Z. Zhang*
Plasmon resonance: Photocatalytic
films of ZnO coated with ultrathin (2
nm) Pt (see figure) are prepared by
a sputtering method, and the Pt/ZnO
films show an efficient visible-light pho-
toresponse for the decomposition of
gas-phase methanol owing to the
unique surface plasmon resonance of
the Pt film.
&& – &&
Reactive Sputtering of Plasmonic Pt/
ZnO Films for Decomposition of Gas-
Phase Methanol under Visible Light
ꢁ
2014 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
ChemPlusChem 0000, 00, 1 – 5
&
6
&
ÞÞ
These are not the final page numbers!