Ultralong Ternary PtRuTe Mesoporous Nanotubes Fabricated by Micelle Assembly with a Self-Sacrificial Template

Article abstract of DOI:10.1002/chem.201806382

High surface area and fast mass transport rate are important to enhance the activity and stability of catalysts. In this work, tellurium nanowires and F127 triblock copolymer are used as self-sacrificial and soft templates, respectively, to synthesize PtR

Full text of DOI:10.1002/chem.201806382

A Journal of
Accepted Article
Title: Ultralong Ternary PtRuTe Mesoporous Nanotubes Fabricated by
Micelle-Assembly with Self-Sacrificial Template
Authors: Shuli Yin, Hongjing Wang, Kai Deng, Zechuan Dai, Ziqiang
Wang, You Xu, Xiaonian Li, Hairong Xue, and Liang Wang
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To be cited as: Chem. Eur. J. 10.1002/chem.201806382
Link to VoR: http://dx.doi.org/10.1002/chem.201806382
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Ultralong Ternary PtRuTe Mesoporous Nanotubes Fabricated by
Micelle-Assembly with Self-Sacrificial Template
Shuli Yin, Hongjing Wang,* Kai Deng, Zechuan Dai, Ziqiang Wang, You Xu, Xiaonian Li, Hairong Xue*,
and Liang Wang*
Abstract: High surface area and fast mass transport rate are
important to enhance the catalytic activity and stability of catalysts.
In this work, tellurium nanowires (Te NWs) and F127 are used as
self-sacrificial template and soft template, respectively, to synthesize
PtRuTe mesoporous nanotubes (PtRuTe MNTs). The designed
PtRuTe MNTs show uniformly distributed mesoporous and internally
hollow structure, which can effectively improve the Pt utilization, the
catalytic activity and durability, and CO tolerance for methanol
oxidation reaction. Very different from the previous 1D metallic
catalysts with solid interiors and smooth surface, the PtRuTe MNTs
are unique in its mesoporous exterior with hollow interior. The
present facile route is very feasible for fabricating 1D mesoporous
metallic catalysts.
Tailoring of the morphology and structure offers an
important approach to enhance catalytic performance of Pt-
based catalysts.[27-31] Various Pt-based nanomaterials with
different morphology have been reported, such as nanoparticles,
nanowires, nanofilms, and nanoflowers, exhibiting the excellent
performance in electrochemical application.[32-35] Benefiting from
the physical and chemical characters, the 1D nanomaterials
have attracted widespread attention.[36,37] 1D Pt-based
nanomaterials show high efficiency of charge transportation,
easy exposure of active sites and anisotropy of morphology,
which is conducive to improving catalytic performance.[38-42]
Electrodeposition method, electrospinning method and template
method are the common approaches for the preparation of 1D
nanomaterials.[43,44] Yamauchi group has reported 1D
mesoporous Pt nanorods by electrodeposition method in a
porous polycarbonate membrane.[44] However, the obtained 1D
nanomaterials prepared by electrodeposition or electrospinning
method commonly show the solid interiors. Among the various
methods, template method is a flexible and effective strategy. At
present, Te, Se, Cu or Ag nanowires (NWs) are used as hard
templates to fabricate tubular nanostructures by galvanic
replacement reaction.[45-47] As a promising sacrificial template,
Te NW favors the fabrication of Pt-based tubular nanomaterials,
because of its easy synthesis, long-term air stability, and high
reactivity.[48] Despite extensive 1D Pt-based nanomaterials have
been reported, most of them show the smooth surface.[49-51]
Owing to large accessible surface area, efficient mass transport
capacity, and more active sites, mesoporous nanostructures
exhibit excellent catalytic properties in various electrochemical
applications.[52-55] Therefore, the fabrication of 1D Pt-based
tubular nanomaterials with mesoporous structures is expected to
enhance catalytic performance for MOR. It is highly desired to
develop a simple and effective method for preparing 1D Pt-
based mesoporous nanotubes.
Introduction
Direct methanol fuel cells (DMFCs) have been attracted a great
attention for a long time, because of the advantages in
environmental protection and energy conversion. Methanol
oxidation reaction (MOR) is crucial to DMFCs, developing high-
efficiency, stabilized, and economical electrocatalysts for MOR
is important to the broad deployment and widespread
commercialization of DMFCs.[1-6] As is well-known, platinum (Pt)
nanomaterials are significant catalysts owing to their outstanding
performance in catalyzing MOR.[7-14] However, the high cost, low
utilization and incident CO poisoning of Pt materials hinder their
development.[15-19] Great efforts have been devoted to
developing promising Pt-based catalysts, such as reducing
catalyst expense, combining with transition metals, and
modifying electronic structure.[20-23] Introducing Pt with other
element is an effective strategy to form more active sites as well
as improve the catalytic activity and stability of Pt-based
catalysts, due to the modulation of its electronic structure
together with the caused lattice strain.[24,25] During the MOR
process, the intermediate COads easily covers on the catalyst
surface and then blocks active site. Thus, it is vital to desorb
COads from the surface. The Ru atoms can reduce the water
dissociation potential, which are recognized as a water activator,
offering more OHads to speed the removing of COads by oxidizing
it to CO2.[26] Therefore, the development of the Ru-introduced Pt
nanomaterials is meaningful to achieve the enhanced catalytic
performance for MOR.
Inspired by this idea, we design and fabricate ultralong
ternary PtRuTe mesoporous nanotubes (PtRuTe MNTs) through
a dual-template method, in which Te NWs and F127 micelles
serve a self-sacrificial template and a pore-forming agent,
respectively. The advantages of morphology boost the catalytic
activities to a great extent. Furthermore, the PtRuTe MNTs show
great synergic effects due to the interaction between each
component. The synthesized ternary PtRuTe MNTs exhibit
superior activity, durability and CO tolerance for MOR.
Results and Discussion
[a] S. Yin, Dr. H. Wang, K. Deng, Z. Dai, Dr. Z. Wang, Dr. Y. Xu, Prof. X. Li, Dr.
H. Xue, Prof. L. Wang
The ultralong PtRuTe MNTs were prepared through a dual-
template strategy in an aqueous solution at room temperature
(Scheme 1). During the synthetic process, the ultralong Te NWs
as self-sacrificial templates show uniform size, large aspect ratio
and high yield, which favor the formation of the high-quality 1D
State Key Laboratory Breeding Base of Green-Chemical Synthesis
Technology, College of Chemical Engineering, Zhejiang University of
Technology, Hangzhou 310014, Zhejiang (China)
E-mails: hjw@zjut.edu.cn, xuehairong@zjut.edu.cn, wangliang@zjut.edu.cn
Supporting information for this article is given via a link at the end of the
document.
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Scheme 1. Schematic illustration of fabrication of the PtRuTe MNTs.
PtRuTe with a hollow tube-like structure (Figure S1). As a soft
template, F127 is conducive to forming the mesoporous
architecture on the surface of the PtRuTe nanotube. It can be
found that the obtained PtRuTe MNTs with uniform size are high
yield, whose average diameter is about 100 nm (Figure 1a). As
shown in Figure 1b, there are plentiful mesopores (~20 nm in
diameter) with a uniform distribution over the entire PtRuTe
MNTs surface. Notably, a distinct nanotubular structure is
observed by the scanning electron microscope (SEM) image for
the cross section (inset of Figure 1b). Transmission electron
microscopy (TEM) image further confirms the nanotubular
structure within the PtRuTe MNTs (Figure 1c). The tube wall of
the PtRuTe MNTs consists of abundant nanoparticles (~5 nm in
diameter) proved by high-resolution TEM (HRTEM) (Figure 1d).
The lattice fringes on the nanocrystals are attributed to the (111)
planes of face-centered cubic (fcc) PtRuTe crystals, because the
measured lattice distance is 0.22 nm (Figure 1d). The concentric
annulus of the selected-area electron diffraction (SAED) pattern
are assigned to the (111), (200), (220), and (311) facets of
metallic fcc structure, which further demonstrates the
polycrystalline structure of the PtRuTe MNTs (Figure S2). X-ray
diffraction (XRD) analysis is used to further explore the metallic
fcc structure of PtRuTe MNTs (Figure S3). There are four
diffraction peaks in the XRD profile of PtRuTe MNTs,
corresponding to the facets of fcc metal, which is in accordance
with the result of SAED pattern. Moreover, these diffraction
peaks have a slight shift relative to those of the standard Pt
peaks (JCPDS card no. 04-0802), because of the incorporation
of the Ru and Te atoms into the Pt lattice.
The structure of PtRuTe MNTs is further confirmed by the
high-angle annular dark-field scanning TEM (HAADF-STEM)
(Figure 2a). It can be seen that the penetrating pores are
uniformly distributed on the surface of a single PtRuTe MNT.
Furthermore, the tubular structure can be clearly distinguished
from the bright and clear contrast of the image. The elemental
mapping images show Pt, Ru and Te elementals uniformly
distribute over the whole nanotube (Figure 2b). Based on the
line-scan profile on the position of white arrow, the formation of
PtRuTe nanotube is confirmed (Figure 2c). Energy-dispersive X-
ray spectrum (EDS) further confirms the existence of Pt, Ru and
Te elementals (Figure 2d).
Figure 1. a, b) SEM images, c) TEM image, and d) HRTEM image of the
PtRuTe MNTs. The inset of (b) shows SEM image of the cross section of the
PtRuTe MNTs. The inset of (d) display Fourier filtered lattice fringe image of
the square area and corresponding FFT pattern.
the products is serious (Figure S4a). In the case that tri-block
copolymer F127 is replaced by bi-block copolymer Brij 58 under
the typically synthetic condition, although the tubular structure
can be obtained, but there is no mesopores structure on the
surface of the PtRuTe nanotubes (Figure S4b). The above
results reveal that F127 is necessary in the synthesis process of
the PtRuTe MNTs, because F127 can serve as not only an
essential dispersing agent but also a soft template for forming
mesoporous structure. In order to ascertain the optimal ratio of
Pt/Ru to fabricate the PtRuTe MNTs, different ratios of Pt/Ru
precursors are introduced into reaction solution. Without adding
Ru precursor, the desired nanotubes with mesoporous structure
can be obtained, named PtTe MNTs (Figure S5a). When the
ratio of Pt/Ru is 3/1, the well-defined PtRuTe MNTs are formed
(Figure S5b). However, the ratio of Pt/Ru is adjusted to 2/2 or
1/3, only the nanotubes with thin-wall can be obtained, and no
mesopores are found on the nanotube surface (Figure S5c-d).
These results indicate that the optimal Pt/Ru ratio for preparing
the PtRuTe MNTs is 3/1.
According to the results of above comparative experiments,
a possible formation process of the PtRuTe MNTs can be
speculated. During the preparation process, Te NW with 1D
structure acts as a hard template to fabricate ternary PtRuTe
MNT. As an important reducing agent, the natural reducibility of
Te NWs facilitates the synthesis of target products through
galvanic replacement reaction. In the galvanic replacement
2-
reaction, the PtCl4 and Ru3+ are readily reduced to Pt and Ru
by Te NWs, respectively, as described in the following equation.
Because of the galvanic replacement reaction partly consumes
the Te NWs, hollow interior of the PtRuTe MNTs are formed.
2PtCl42- + Te + 3H2O → 2Pt + TeO32- + 8Cl- + 6H+ (1)
To investigate the roles of synthetic factors for the PtRuTe
MNTs, a series of comparative experiments are performed.
When no surfactant is added, only tubular nanomaterials with
nonuniform morphology are obtained, and the agglomeration of
4Ru3+ + 3Te + 9H2O → 4Ru + 3TeO32- + 18H+
(2)
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Figure 3. a) ECSA-normalized and b) mass-normalized CV curves of different
catalysts in 0.5 M H2SO4 with 1 M CH3OH at a scan rate of 50 mV s-1. c) The
comparisons of the specific activities and mass activities. d)
chronoamperometric curves (recorded at 0.60 V) obtained in 0.5 M H2SO4 with
1 M CH3OH. The currents densities are normalized by the ECSAs.
Figure 2. a) HAADF-STEM image, b) elemental mapping images, c)
compositional line profiles, and d) EDS spectrum of the PtRuTe MNTs.
Ascorbic acid (AA) is used as a reducing agent along with
Te NWs. The introduction of AA assists the complete reduction
of precursor species, which favors forming well-defined
mesoporous structures.[56] In the absence of AA, there is no
porous structure on the product surface (Figure S6). Except for
Te NWs, F127 plays an indispensable role in the synthesis of
The MOR measurements are performed in 0.5 M H2SO4 and 1.0
M CH3OH electrolyte at a scan rate of 50 mV s-1. In the potential
range between 0.35 to 1.00 V, a distinct methanol oxidation
peak can be detected. The specific activities of different
catalysts are normalized to the ECSAs, which is a significant
argument to estimate the performance in MOR. The specific
activity of the PtRuTe MNTs is 1.89 mA cm-2 at the peak
potential, which is about 1.04 times of the PtTe MNTs (1.82 mA
cm-2) and 3.71 times of Pt/C (0.51 mA cm-2) (Figure 3a). The
mass activities of different catalysts are normalized to the
loading amount of Pt, which can be used to reflect the
performance of catalyst in MOR as well (Figure 3b). The PtRuTe
MNTs, PtTe MNTs, and Pt/C display different mass activities.
The sequence of them is PtRuTe MNTs (0.98 mA µg-1Pt) > PtTe
MNTs (0.83 mA µg-1Pt) > Pt/C (0.22 mA µg-1Pt) (Figure 3c).
These data exhibit that the PtRuTe MNTs have an excellent
catalytic activity for MOR. The specific activity and mass activity
of the PtRuTe MNTs are also higher than the previously
reported Pt-based catalysts (Table S1). The accelerated
durability test is carried out to research the stability of the
samples in the MOR process, using CV in 0.5 M H2SO4 and 1.0
M CH3OH electrolyte (scan rate: 50 mVs −1). After 2,000 cycles,
the specific activities of the PtRuTe MNTs, PtTe MNTs, and Pt/C
decrease to some extent. The retention of specific activity of
PtRuTe MNTs is 84.7 %, which is more stable than PtTe MNTs
(82.2 %) and Pt/C (71.2 %) (Figure S8). The stability of different
samples is measured by chronoamperometry for 3,600 s at 0.6
V (Figure 3d). The PtRuTe MNTs show a slower degenerative
current density during the testing time, indicating its better
stability for MOR relative to the PtTe MNTs and Pt/C. The above
results indicate that introducing Ru into Pt can enhance the
catalytic performance. In addition, we also prepared PtRu MNTs
mesoporous structures. F127 is triblock copolymer (PEO100
-
PPO70-PEO100), the center is hydrophobic polypropylene oxide
(PPO) and the ends are hydrophilic polyethylene oxide (PEO)
chains. The hydrophilic end (PEO) facilitates the adsorption of Pt
and Ru precursor species, and the reduced Pt can be deposited
on the spherical soft template (F127 micelles).[57,58] During the
atomic addition process, the selected factors together with the
optimized Pt precursor amounts facilitate the formation of the
PtRuTe MNTs.
The PtRuTe MNTs are estimated as the MOR catalyst, and
benchmarked against the PtTe MNTs and commercial Pt/C (20
wt% Pt). The atomic ratios of the Pt/Ru/Te for the PtRuTe MNTs
and Pt/Te for the PtTe MNTS are about 47.3/19.1/33.6 and
68.3/31.7, respectively, detected by the inductively coupled
plasma mass spectrometry (ICP-MS) analysis. Cyclic
voltammetries (CVs) are carried out to reveal the surface
property of different catalysts in 0.5 M H2SO4 at a scan rate of
50 mV s−1 (Figure S7). The hydrogen adsorption peak and
desorption peak can be distinctly observed in CVs.
Electrochemical surface area (ECSA) of different samples is
calculated based on the hydrogen desorption peak of CVs. After
calculation, the ECSA values of PtRuTe MNTs, PtTe MNTs, and
Pt/C are 50.2, 45.0, and 43.0 m2 g-1, respectively. Obviously, the
PtRuTe MNTs possess the higher ECSA than PtTe MNTs,
because of the introduction of Ru species. In addition, the ECSA
of the PtRuTe MNTs is higher than that of the Pt/C, owing to the
well-organized 1D tubular structure and mesoporous structure.
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structure, the as-prepared PtRuTe MNTs possess mesoporous
structure which can effectively increase the active site and
facilitate mass diffusion. The advantages of morphology and
composition of PtRuTe MNTs contribute to the improvement of
catalytic activity, durability and CO tolerance for MOR. The
develped synthetic method is highly vaulable to synthesize
binary and ternary Pt-based mesoporous tubular catalysts.
Figure 4. a) CO stripping voltammograms, b) locally amplified CO stripping
voltammograms in 0.5 M H2SO4 at a scan rate of 50 mV s-1.
Experimental Section
Chemicals and Materials
by etching PtRuTe MNTs and chose PtRu MNTs as
a
Na2TeO3 (99.9%), NH3·H2O, N2H4·H2O (98%), polyvinylpyrrolidone (PVP,
58000), ascorbic acid (AA), acetone and HCl were purchased from
Aladdin. Pluronic F127, K2PtCl4, RuCl3 and Nafion 117 solution (5 wt %)
were bought from Sigma-Aldrich. Commercial Pt/C (20 wt% Pt) was
obtained from Alfa Aesar Co.
comparison. The PtRu MNTs have the similar catalytic activity
and slightly poor stability relative to PtRuTe MNTs (Figure S9
and Figure S10), owing to some breakage of the nanowires
(Figure S11). This result shows that the presence of Te
facilitates the preserving of its intact tubular structure, which
favors the improvement of its catalytic performance.
Synthesis of Te nanowires
In order to examine the resistance to CO of different
catalysts, the CO stripping tests for the samples are conducted
in 0.5 M H2SO4 solution (scan rate: 50 mV s-1) (Figure 4a).
Because of the oxidation of the CO absorbed on the catalyst
surfaces, a sharp peak can be detected. It is noted that the CO
oxidation peak of the PtRuTe MNTs (0.621 V) locates more
negative than those of the PtTe MNTs (0.660 V) and Pt/C (0.704
V), indicating the good CO tolerance ability (Figure 4b).
Benefitting from the advantages of component, mesoporous
structure and tubular structure, the PtRuTe MNTs display the
high electrocatalytic activity and durability for MOR. Te is
conducive to maintaining its intact tubular structure, and the
presence of Te effectively reduces the Pt content in the
nanomaterials. Owing to the presence of mesoporous structure,
the surface area and active sites are increased, and the diffusion
of the reactants and the infiltration of the electrolyte can be
effectively improved. Moreover, ultralong hollow continuous
nanotubular framework improve the Pt utilization, increases
electron transfer rate, reduces diffusion resistance, and makes
full use of the interior and exterior surfaces of the nanomaterial.
The introducing Ru into Pt can modulate the electronic structure
of the Pt, which is beneficial to the cleavage of the C–H bond
within CH3OH molecules at lower potentials. Moreover, the
strain effect caused by the lattice mismatch between Pt and Ru
atoms can reduce the binding energies of reaction intermediates,
which leads to a high CO-tolerance.
Te NWs were synthesized according to the traditional synthesis method
with a little modification.[59] Specifically, Na2TeO3 (0.092 g) and PVP (1 g)
were added to H2O (35.22 mL) and stirred strongly at ambient conditions
until completely dissolved. And then, N2H4·H2O (1.43 mL) and NH3·H2O
(3.35 mL) were mixed with above solution and shaken evenly.
Subsequently, the obtained solution was heated to 180 °C and
maintained 3 h in 50 mL reaction kettle. Finally, the production was
dispersed in acetone, and Te NWs were collected by
centrifugation/washing cycles three times with water. The obtained Te
NWs were dissolved in H2O (15 mL) for further use.
Synthesis of PtRuTe MNTs
The PtRuTe MNTs were prepared using a simple method. Typically,
K2PtCl4 (1.5 mL, 20 mM), RuCl3 (0.5 mL, 20 mM), HCl (0.02 mL, 6 M)
and F127 (20 mg) was mixed uniformly under sonication. Then, Te NWs
(0.2 mL) and AA (2 mL, 0.1 M) were added. The mixture was slowly
magnetic stirred for 2 h at room temperature. Finally, PtRuTe MNTs were
obtained by centrifugation at 5,000 rpm for 10 min and washed with
water three times.
Materials Characterization
Scanning electron microscope (SEM) was determined by Hitachi S-4800
with an acceleration voltage of 5 kV. A JEOL-2100F with an energy-
dispersive X-ray spectroscopy (EDS) was used to investigate
transmission electron microscopy (TEM), high-resolution TEM (HRTEM)
and element mappings operated at 200 kV. The X-ray diffraction (XRD)
was carried out on a Rigaku Miniflex 600 performed at 15 mA current and
40 kV accelerating voltage. ICP-MS analysis was carried out on an Elan
DRC-e instrument.
Conclusions
Electrochemical measurements of MOR
In summary, well-defined ternary PtRuTe mesoporous
nanotubes are successfully synthesized by a facile method. The
Te NWs induce the formation of tubular structure by galvanic
replacement reaction, while F127 micelles serve as soft
template for the fabrication of mesoporous structure. Moreover,
introducing Ru species is beneficial to enhance MOR
performance. Different from previously reported Pt-based tubular
A CHI 660D electrochemical analyzer was used to investigate the MOR
electrochemical properties of the catalysts. To set up a traditional three-
electrode system, glassy carbon electrode with diameter of 3 mm and Pt
wire were used as working electrode and counter, respectively, and
Ag/AgCl was used as reference electrode. Before prepare working
electrode, the glassy carbon electrode was furbished with Al2O3 powder
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and cleaned with water. All the catalysts were diluted to a concentration
of 2 mg mL-1. The working electrode was modified by 2 μg of sample
attributing to Pt. After desiccation, the surface of catalysts was coated
with Nafion (2 μL, 0.5 %) served as binder and dried at room temperature.
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Four in one: Tellurium nanowires and
F127 are used as self-sacrificial
Shuli Yin, Hongjing Wang,* Kai Deng,
Zechuan Dai, Ziqiang Wang, You Xu,
Xiaonian Li, Hairong Xue,* and Liang
Wang*
template
and
soft
template,
respectively, to synthesize PtRuTe
mesoporous nanotubes for methanol
oxidation reaction.
Page No. – Page No.
Ultralong
Ternary
PtRuTe
Mesoporous Nanotubes Fabricated
by Micelle-Assembly with Self-
Sacrificial Template
This article is protected by copyright. All rights reserved.