Journal of the Taiwan Institute of Chemical Engineers 70 (2017) 161–167

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Journal of the Taiwan Institute of Chemical Engineers

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

Hydrogen production by photocatalytic water-splitting on Pt-doped

TiO2 –ZnO under visible light
Meng-Yu Xie a, Kang-Yang Su a, Xin-Yuan Peng a, Ren-Jang Wu a,∗, Murthy Chavali b,
Wei-Chen Chang c
a
Department of Applied Chemistry, Providence University, Shalu, Taichung 43301, Taiwan, ROC
b
CoExAMMPC and Division of Chemistry, Department of Sciences and Humanities, Vignan’s Foundation for Science, Technology and Research University
(VFSTR) University; Vignan’s University, Vadlamudi, Guntur 522 213, Andhra Pradesh, India
c
Institute of Nuclear Energy Research, Atomic Energy Council, 1000 Wenhua Rd., Chiaan Village, Lungtan, Taoyuan 325, Taiwan, ROC

a r t i c l e i n f o a b s t r a c t

Article history: Pt/TiO2 –ZnO photocatalytic materials were prepared for the generation of hydrogen gas from water split-
Received 4 June 2016 ting. The photocatalysts were characterized by X-ray diffraction (XRD), UV-visible spectra (UV–Vis), scan-
Revised 8 October 2016
ning electron microscope (SEM) and transmission electron microscope (TEM). The absorption wavelength
Accepted 20 October 2016
of TiO2 was shifted to longer wavelength on Pt/TiO2 –ZnO. A 400 W mercury arc lamp with a cutoff filter
Available online 1 November 2016
which filter out all the wavelengths under 400 nm as the visible light source. It reached up to the opti-
Keywords: mum value of 203 μmolh−1 g−1 on TiO2 –ZnO (Ti/Zn = 10). A catalyst of 0.5 wt% Pt/TiO2 –ZnO (Ti/Zn = 10)
Photocatalysts was used and a best hydrogen production rate through water splitting was reaching to 2150 μmolh−1 g−1 .
Pt/TiO2 –ZnO The 0.1 wt% Pt/TiO2 –ZnO showed a satisfying long-term stability, and 88% and 77% of initial hydrogen
Hydrogen production productivity still remained after 7 days and 14 days, respectively.
© 2016 Taiwan Institute of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

1. Introduction For the past few years, the photocatalysis [7–10] activity has
been studied with some semiconducting metal oxides like TiO2 [7],
The main renewable energy sources are solar energy, wind, wa- ZnO [8], WO3 [9], SnO2 [10], and Ta2 O5 [11]. They become com-
ter, and biomass. The biomass is the other energy source below monly studied and hot photocatalysis material. Photocatalysis takes
the petroleum, the gas, the coal. It provides about 11% of the basic wavelength energy of photo in special wavelength shining. The
energy demand and 88% of applying for a global renewable energy electron is stirred up from valence band to conductance band; the
source. The hydrogen energy source of the biomass, has a variety excitation electron and electron hole resolve the water to hydrogen
of recycling and clean, is thought one kind of perfect and have the [7]. Some scholars focused the visible light as the light source to
potential of energy source [1]. the water splitting reaction for the sake of there are near 50% visi-
There are many ways to produce hydrogen, such as solar en- ble light from the sun. TiO2 nanotubes possess many benefits such
ergy pyrogenic decomposition [2], photo-electrochemistry method as providing unidirectional electric channel, large specific surface
[3], photocatalytic method, [4] and solar energy combination with area, high yield of energy conversion and single-step synthesis for
electrolytic process [5,6]. In 1972, a phenomenon for hydrogen pro- preparation [12–14]. To improve the hydrogen yields, metal oxides
duction from photodecomposition of water on TiO2 electrode was composites or low cost metals addition are attempted to dope on
discovered [3]. It was found that when ultraviolet light irradiating TiO2 nanotubes [15–26]. It obtained a very high promotion on hy-
on TiO2 , the electron is excited from the valence band to conduc- drogen evolution of water splitting reaction [12–27]. The photocat-
tion band, then the exciting electron form anode of TiO2 moves to alyst of SrTiO3 possessed photocatalytic activity for water splitting
the cathode of Platinum, let the water resolve and hydrogen pro- under visible light thereby produced the average rate of H2 evolu-
duce. This display that the possibility to translate from solar energy tion of 122.6 μmol h−1 [28]. A water splitting performance based
to chemical energy. Now, the decomposition water to produce hy- on H2 generation photocatalyst of TiO2 /C3 N4 , and obtained a hy-
drogen gas turns into an important technology in the world [6]. drogen production as 50.2 μmoh−1 [29]. The mesoporous Pt/TiO2
photocatalyst prepared by the single step sol-gel method showed
higher photocatalytic activity for H2 evolution of 0.6 wt% Pt load-
∗
Corresponding author. Fax: +886426327554. ing content and got a hydrogen production to 1400 μmoh−1 g−1
E-mail addresses: [email protected], [email protected] (R.-J. Wu). [30]. The visible light photocatalytic activity of water splitting

http://dx.doi.org/10.1016/j.jtice.2016.10.034
1876-1070/© 2016 Taiwan Institute of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
162 M.-Y. Xie et al. / Journal of the Taiwan Institute of Chemical Engineers 70 (2017) 161–167

Fig. 1. Equipment setup for the photocatalytic H2 evolution by water splitting reaction.

reaction towards hydrogen production was promoted by Pt/N-TiO2 , all samples was examined in 250 mL methanol aqueous solution
and the hydrogen yield is obtained to 772 μmoh−1 g−1 [31]. The (10% methanol by volume) containing 0.5 g photocatalyst under
TiO2 –ZnO mixed oxides photocatalysts were prepared by the sol- magnetic stirring at 25 °C. Methanol was used in the solution
gel method and used for the H2 production from water splitting, as a sacrificial reagent which scavenges photo-generated holes. A
and the hydrogen yield is obtained to 1300 μmoh−1 [32]. 400 W mercury lamp with UV cut filter (>400 nm) was used as the
In this study, the addition of ZnO to TiO2 by a sol–gel method light source [33]. Before irradiation, the system was thoroughly de-
then uses impregnation method to add Pt on to form Pt/TiO2 – gassed in order to remove air. The gaseous products were analysed
ZnO. No researcher has used the catalyst of Pt/TiO2 –ZnO. A 0.5 wt% by an on-line gas chromatography (Gas Chromatography Personal
Pt/TiO2 –ZnO (Ti/Zn = 10) was used and a best hydrogen production GC 10 0 0, China) equipped with a packed column (MS-5A, 3 m in
rate through water splitting was reaching to 2150 μmolh−1 g−1 . length) and a TCD detector, using Ar as the carrier gas [33]. In ad-
dition, each experiment was carried out at least three times.
2. Experimental
2.3. Photo-electrochemical measurement
2.1. Preparation of photocatalysts
For photocurrent measurements, the electrodes were immersed
The photocatalysts of TiO2 (ST21) and ZnO were purchased by in a solution of 1 M NaOH. The working electrode was scanned
commercial company, TiO2 –ZnO and Pt/TiO2 –ZnO were prepared from −0.1 to 0.7 V (versus Ag/AgCl electrode) at a rate of 1 mV/s.
by followings in our lab. 0.34 g Zinc sulphate (ZnSO4 ), 18 ml D.I. The TiO2 , TiO2 –ZnO and 0.5% Pt/TiO2 –ZnO samples coated on
water and 40 ml methanol (CH3 OH) were mixed to form a solu- working electrodes were illuminated with a 400 W mercury lamp
tion, then added appropriate amounts of aqua ammonia (NH4 OH) with UV cut filter (>400 nm), and it was used as the light source.
to adjust the pH value to 9. Then 10 ml tetra butyl ortho titanate
Ti(C4 H9 O)4 was added, and stirred for three hours become white 2.4. Characterised by XRD, UV–Vis and TEM
colloid, and next heat with 70 °C stirring until it becomes powder.
Take this powder into bake oven for two hours, then grind sample The photocatalytic samples were analysed by powder X-ray
ball for eight hours. Put the sample in the oven and calcined at diffraction spectra using an XRD-60 0 0 Shimadzu X-RAY Diffrac-
500 °C for 2 h, and it will get the sample of TiO2 –ZnO (Ti/Zn = 10). tometer, with Cu Kα radiation (Cu Kα 1, 1.54060 Å) at 35 kV and
Various ratios of Ti/Zn photocatalyst blended material can be ob- 35 mA between 10º and 80º (2θ ) with 2º / min. Spectroscopy Ultra-
tained as following the same process. violet (UV)-Vis absorption spectra were obtained using a UV–Vis
By taking 1 g TiO2 –ZnO, 30 ml methanol and appropriate spectrometer (UV-2550, Shimadzu, Japan). The surface morphology
amounts of chloroplatinic acid (H2 PtCl6 ·6H2 O) into the aqueous so- of all samples were characterized by field emission scanning elec-
lution, stir it continuously for three hours, heat with 70 °C and stir tron microscopy (JEOL JEM-2100F). The elemental composition was
continue until it becomes powder, put in bake oven for two hours, determined by energy dispersive X-ray spectroscopy (EDX) and el-
grind sample ball for eight hours. Next to put it in 300 °C calcina- emental mapping. Transmission electron microscopy (TEM) images
tion for two hours, the various platinum weight ratio percentage were taken using JEOL JEM-2100F. All the characterization samples
(wt%) of Pt/TiO2 –ZnO photocatalytic samples were obtained. of TiO2 –ZnO is fixed at Ti/Zn = 10.

2.2. Water splitting system 3. Results and discussion

It showed a schematic diagram of the experimental arrange- 3.1. Characterization of the catalysts using XRD, TEM and UV–Vis
ment used for the water splitting reaction in the production of hy-
drogen in Fig. 1 [31,33]. Photocatalytic reactions were conducted The XRD patterns of TiO2 , TiO2 –ZnO, 3.0 wt% Pt/TiO2 –ZnO and
in a Pyrex glass reactor that contained with a cooling water sys- ZnO are shown in Fig. 2(a), (b), (c) and (d), respectively. Diffraction
tem. Photocatalytic activity measurement hydrogen production of peaks that are attributable to anatase TiO2 are clearly observed in
 M.-Y. Xie et al. / Journal of the Taiwan Institute of Chemical Engineers 70 (2017) 161–167 163

Fig. 2. XRD spectra of (a) TiO2 , (b) TiO2 –ZnO, (c) 3.0 wt% Pt/TiO2 ––ZnO, (d) ZnO.

the samples of Fig. 2(a), (b) and (c), which are in good accordance
with those in the standard JCPSD cards No.21-1272. In addition, the
pattern for the all samples exhibit diffraction peaks appeared at
2θ = 25.28º, 37.80º, 48.05º, 53.89º, 62.69º and 75.03º corresponding
to (101), (0 04), (20 0), (105), (204) and (215) planes can be seen.
It should be noted that the deposited Pt do not affect the crys-
tal structure of anatase TiO2 and one distinct additional diffraction
peak of metallic Pt is found in Fig. 2(c). Fig. 2(c) revealed the peak
at 39.76º attributed to Pt (111) plane are apparently observed in the
XRD patterns. Fig. 2(d) presented the ZnO sample exhibit diffrac-
tion peaks appeared at 2θ = 31.77º, 34.42º, 36.25º and 47.54º corre-
sponding to (100), (002), (101), and (102) planes can be seen.
In order to examination the morphology of TiO2 –ZnO and
0.5 wt% Pt/TiO2 –ZnO, SEM images and EDX spectra were com-
pleted, which are showed in Fig. 3(a), (b) and (c) and Fig. 4(a), (a)
and (c). It can be found that TiO2 –ZnO shows non uniform-shape
of Fig. 3(a) in micrometer scale. From Fig. 3(b) and (c), it can be
observed that the Ti, O, Zn and C were observed in the EDX spec-
trum and elemental mapping of the TiO2 –ZnO. Fig. 4(a) revealed
some sphere-like structure on the surface of 0.5 wt% Pt/TiO2 –ZnO.
In Fig. 4(b) and (c), it can be observed that the Ti, O, Zn, Pt and C
were observed in the EDX spectrum and elemental mapping of the
0.5 wt% Pt/TiO2 –ZnO.
The TEM images of TiO2 , ZnO and 0.5 wt% Pt/TiO2 –ZnO are
shown in Fig. 5(a), (b) and (c), respectively. Fig. 5(a) showed a set
of regular lattice fringes of 0.36 nm is consistent with the (101)
crystal plane of the TiO2 . A lattice fringe of 0.26 nm is consistent
with the (002) crystal plane of the ZnO in Fig. 5(b). It can be iden-
tified that there are TiO2 (101) d = 0.36 crystal form and Pt (111)
d = 0.22 crystal form, but there is no ZnO crystal form in Fig. 5(c).
The possible microstructure of TiO2 –ZnO blended material is TiO2
dispersed on ZnO surface, so it can’t form crystal structure by XRD
(Fig. 2(b) and (c)) and TEM (Fig. 5(c)) [32].
In order to research the optical absorption properties of the
photocatalysts, the UV-visible absorption spectra of TiO2 , ZnO,
TiO2 –ZnO and 0.5 wt% Pt/TiO2 –ZnO were investigated in Fig. 6(a),
(b), (c) and (d). Fig. 6(a), (b) and (c) present the absorption spec-
tra of ZnO, TiO2 and TiO2 –ZnO, respectively. It is seen that the ZnO
and TiO2 –ZnO possess longer wavelength absorption than TiO2 in
Fig. 6(a), (b) and (c). In Fig. 6(d), 0.5 wt% Pt/TiO2 –ZnO shows a
Fig. 3. (a) SEM images of TiO2 –ZnO, (b) EDX layered images of TiO2 –ZnO, (c) ele-
strongest photoabsorption in the visible light region (wavelength mental EDX mapping of TiO2 –ZnO.
>430 nm). In addition, the band gap was calculated from the UV-
visible absorption spectra (Table 1). Table 1 presents the band gap
164 M.-Y. Xie et al. / Journal of the Taiwan Institute of Chemical Engineers 70 (2017) 161–167

Fig. 4. (a) SEM images of 0.5% Pt/TiO2 –ZnO (b) EDS layered images of 0.5% Pt/TiO2 –
ZnO (c) elemental EDX mapping of 0.5% Pt/TiO2 –ZnO.

Table 1
Band gap of various photocatalysts.

Catalysts Band gap (eV)

TiO2 3.23
ZnO 3.02
TiO2 –ZnO (Ti/Zn = 10) 3.18
Pt/TiO2 –ZnO (Ti/Zn = 10) 3.08 Fig. 5. TEM images of (a) TiO2 , (b) ZnO, (c) 0.5%Pt/TiO2 –ZnO (Ti/Zn = 10).
 M.-Y. Xie et al. / Journal of the Taiwan Institute of Chemical Engineers 70 (2017) 161–167 165

Fig. 6. Reflective spectra of UV visible (a) ZnO (b) TiO2 (c) TiO2 –ZnO (d) 0.5 wt% Pt/TiO2 –ZnO.

Table 2
Hydrogen gas yield of various Ti/Zn ratios of TiO2 –ZnO pho-
tocatalysts.

Catalyst Hydrogen yield (μmolh−1 g−1 )

TiO2 68
ZnO 3.0
Ti/Zn = 2 83
Ti/Zn = 4 107
TiO2 –ZnO Ti/Zn = 6 144
Ti/Zn = 8 171
Ti/Zn = 10 203
Ti/Zn = 12 152

Table 3
Hydrogen yield of various Pt loadings on TiO2 –ZnO (Ti /
Zn = 10).
Fig. 7. Hydrogen yield versus reaction time of various Pt loadings on TiO2 –ZnO (Ti /
Catalyst Hydrogen yield (μmolh− 1 g− 1 )
Zn = 10): (a) 0.01 wt% Pt/TiO2 –ZnO, (b) 0.05 wt% Pt/TiO2 –ZnO, (c) 0.1 wt% Pt/TiO2 –
TiO2 –ZnO 203 ZnO, (d) 0.5 wt% Pt/TiO2 –ZnO, (e) 1.0 wt% Pt/TiO2 –ZnO.
0.01 wt% Pt/TiO2 –ZnO 916
0.05 wt% Pt/TiO2 –ZnO 1313
0.1 wt% Pt/TiO2 –ZnO 1789
0.5 wt% Pt/TiO2 –ZnO 2150 and 1789 μmolh−1 g−1 , respectively after 300 min. The reason is
1.0 wt% Pt/TiO2 –ZnO 820
that the photocatalytic reaction reached equilibrium. On another
way to understand the Pt promotion effect on TiO2 –ZnO to wa-
ter splitting reaction. It can be achieved by photocurrent measure-
values of commercial TiO2 , ZnO, TiO2 –ZnO and 0.5 wt% Pt/TiO2 – ments in Fig. 8, the TiO2 , TiO2 –ZnO and 0.5% Pt/TiO2 –ZnO sam-
ZnO are 3.23 eV, 3.02 eV, 3.18 eV and 3.08 eV, respectively. ples coated on working electrodes were illuminated with a 400 W
mercury lamp with UV cut filter (>400 nm), and it was used as
3.2. Yields of hydrogen generation the light source. Fig. 8(a), (b) and (c) presented the 0.5% Pt/TiO2 –
ZnO electrode can generate most high photochemical current than
Table 2 reveals the hydrogen yields of TiO2 , ZnO and various ra- others.
tios of TiO2 –ZnO samples from water splitting. It can be found that In Table 3, the addition of Pt can increase the hydrogen yield
the hydrogen production rates of TiO2 and ZnO are 68 μmolh−1 g−1 about four to ten times with TiO2 –ZnO. These results prove that Pt
and 3.0 μmolh−1 g−1 , respectively. The hydrogen yields of various can promote the separation efficiency of electron–hole pairs on the
ratios from Ti/Zn = 2 to 12 of TiO2 –ZnO are higher than TiO2 and Pt/TiO2 –ZnO surface, which plays a role of electron transfer inter-
ZnO. It reached up to the optimum value of 203 μmolh−1 g−1 while mediate. Meanwhile, Pt can effectively prevent the direct recombi-
the Ti/Zn = 10. All the TiO2 –ZnO (Ti/Zn = 10) samples with vari- nation of electrons and holes, which retards the electron–hole re-
ous Pt loading from 0.01 wt% to 1.0 wt% exhibited photocatalytic combination rate in water splitting reaction. These two effects may
activity for hydrogen production from water splitting in Table 3 combine and result in a further increment in photocatalytic activ-
and Fig. 7. The optimum Pt loading is 0.5 wt%, and it can achieve ity of Pt/TiO2 –ZnO.
the maximum hydrogen yield to 2150 μmolh−1 g−1 . From Fig. 7, it Every seven days take once determine, finding that the ex-
presented that the hydrogen production rate of 0.5 wt% Pt/TiO2 – periment material has good reproducibility in Fig. 9. The 0.1 wt%
ZnO reached up to a stable yield 2150 μmolh−1 g−1 after 420 min Pt/TiO2 –ZnO showed a satisfying long-term stability, and 88% and
under visible light irradiation. Meanwhile, the hydrogen produc- 77% of initial hydrogen productivity still remained after 7 and 14
tion rate of 0.01 wt% Pt/TiO2 –ZnO, 0.05 wt% Pt/TiO2 –ZnO and 0.1 days, respectively, as illustrated in Fig. 9. Therefore, the Pt/TiO2 –
wt% Pt/TiO2 –ZnO reached up to 916 μmolh−1 g−1 , 1313 μmolh−1 g−1 ZnO was high activity, efficiency and long-term stability.
166 M.-Y. Xie et al. / Journal of the Taiwan Institute of Chemical Engineers 70 (2017) 161–167

Fig. 8. Current-potential curves with chopped light measured in 1 M NaOH with a scan rate of 1 mV s−1 for various samples of (a) TiO2 –ZnO, (b) 0.5% Pt/TiO2 –ZnO, (c) TiO2 .

Fig. 9. Re-use of photocatalysts of 0.1 wt% Pt/TiO2 –ZnO.

3.3. Probable photocatalytic mechanism of the photocatalytic water splitting reaction based on Pt/TiO2 –ZnO
is the Pt deposited on TiO2 structure, and ZnO are surrounded by
A photocatalytic mechanism of splitting water reaction was pro- the structure as shown in Fig. 10(b).
posed by following Eqs. (1)–(5) [30,32,33]. Fig. 10(a) revealed that
when Pt/TiO2 –ZnO is irradiated, an electron may be excited from TiO2 –ZnO → TiO2 –ZnO (e− + h+ ) (1)
the valence band to the conduction band on the TiO2 –ZnO, as
shown in Eq. (1). Simultaneously, it is very likely that some ex- TiO2 –ZnO (e− + h+ ) → TiO2 –ZnO (2)
cited electrons in conduction band can come back to valence band
to recombine with the holes on TiO2 –ZnO according to the Eq. (2). h+ + H2 O → H+ + • OH (3)
Pt nanoparticles were placed on the surface can act as electron
traps and inhibit the hole-electron recombination by accumulating 2e− + 2H+ H2 (4)
the electrons [31–33]. Then, the holes react with H2 O molecules to
•
form the products of H+ and • OH, as designated in Eq. (3). Even- OH + • OH → H2 O + 1/2O2 (5)
tually, the H+ and • OH are reduced and oxidised by the photogen-
erated electrons and holes to produce H2 and O2 , respectively, as H2 O → H2 + 1/2O2 (6)
shown in Eqs. (4) and (5). Eqs. (1), (3), (4) and (5) are summarised
as Eq. (6). 4. Conclusion
Additionally, in a water-splitting reaction Pt is loaded on the
surface as a dispersion of nanoparticles to produce active sites and The photocatalysis of Pt/TiO2 –ZnO for water-splitting which has
accelerate the reduce reaction of H+ to generate hydrogen on Pt in the benefits of preparing easily, environmentally friendly and good
Fig. 10(a) and (b) [30,33]. Furthermore, the probable active centre re-utilization. The optimal experimental conditions, the titanium
 M.-Y. Xie et al. / Journal of the Taiwan Institute of Chemical Engineers 70 (2017) 161–167 167

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