Pt embedded in carbon rods of N-doped CMK-3 as a highly active and stable catalyst for catalytic hydrogenation reduction of bromate

Article abstract of DOI:10.1039/c9cc05274g

A novel Pt-based catalyst with fine and homogeneous Pt particles embedded in carbon rods of N-doped CMK-3 was fabricated by a two-step infiltration method using SBA-15 as the template. Due to its fine particle size, N-containing functionality and effective embedment of Pt particles in carbon rods, the catalyst exhibited superior catalytic activity and stability in the liquid phase catalytic hydrogenation of bromate in water.

Full text of DOI:10.1039/c9cc05274g

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Pt embedded in carbon rods of N-doped CMK-3 as highly active and stable
catalyst for catalytic hydrogenation reduction of bromate
Received 00th January 20xx,
Accepted 00th January 20xx
Minghui Li, Yuan Hu, Heyuan Fu, Xiaolei Qu, Zhaoyi Xu, Shourong Zheng*
DOI: 10.1039/x0xx00000x
uncoated catalysts, metal particles of the coated catalyst were
inaccessible for reactants, while the intimate contact between
embedded metal particles and carbon overcoating resulted in
unique metal-carbon heterojunctions, capable of evoking Mott-
Schottky effect.12 As a result, the carbon layers were activated
and acted as catalytically active sites, on which H2 could be
adsorbed and activated.10,12 Accordingly, enhanced stability of
the coated catalysts was normally achieved at the cost of
catalytic activities due to complete embedment of active metal
particles beneath overcoatings despite of the formation of
active metal-carbon heterojunctions.13,14 Hence, fabrication of
catalysts with both high stability and activity is still highly
challenging.
Mesoporous carbon is generally considered as one of the
best choices as catalyst supports due to its ordered pore
structure, large surface area and accessible pore volume.15
Herein, we report the fabrication of novel catalysts with highly
dispersed Pt particles, which are embedded in the carbon rods
of N-doped mesoporous carbon by a two-step infiltration
method using SBA-15 as the template. In comparison with
typical Pt catalyst coated by nonporous carbon layers
(Pt/CNT@C), Pt catalysts embedded in the carbon rods of
mesoporous carbon and N-doped mesoporous carbon (denoted
as Pt@CMK-3 and Pt@N-CMK-3 respectively) had higher
surface areas. Additionally, Pt@N-CMK-3 had a higher point of
zero charge (PZC) than Pt@CMK-3 and Pt/CNT@C due to the
presence of N-containing functionalities, which was likely
beneficial for the adsorption of anionic pollutants on catalyst
surface. The preparation procedure of the catalysts is illustrated
in Scheme 1 and more synthesis details can be found in the
experimental section of the electronic supplementary
information (ESI†). In a typical procedure, a desired amount of
Novel Pt-based catalyst with fine and homogeneous Pt
particles embedded in carbon rods of N-doped CMK-3 was
fabricated by a two-step infiltration method using SBA-15 as
the template. Due to its fine particle size, N-containing
functionality and effective embedment of Pt particles in
carbon rods, the catalyst exhibited superior catalytic activity
and stability in the liquid phase catalytic hydrogenation of
bromate in water.
Supported precious metal catalysts have been widely used in
liquid phase catalytic hydrogenation under ambient conditions
to remove pollutant, such as nitrate, perchlorate, bromate and
chlorophenols.1-4 However, leaching, aggregation or/and
surface contamination of metal particles inevitably occur,
leading to catalyst deactivation during the catalytic processes.5,6
Numerous attempts have been made to avoid the deactivation
of supported noble metal catalysts. For example, heteroatom
doping (e.g., N-, S- or B-doping) was used to enhance metal-
support interaction of noble metal catalysts supported on
carbonaceous supports in order to alleviate catalyst
deactivation.7,8 Confining metal particles in the pores of zeolite,
MOFs and mesoporous SiO2 was confirmed to effectively
suppress catalyst deactivation.9 Very recently, embedment of
metal particles beneath conductive carbon layers has been
proved to be a prominent strategy to enhance catalyst stability.
For example, Fu et al.10 prepared a coated Ni/Al2O3 catalyst with
N-doped carbon layer, which exhibited a superior stability for
catalytic hydrogenation reduction of 4-nitrochlorobenzene
even under strong acidic conditions. In parallel, Li et al.11
developed a stable and reusable coated carbon nanotube (CNT)
supported Pd catalysts by a N-doped carbon shell and observed
superior sintering resistance and high stability for catalytic
Cr(VI) reduction. In contrast to their counterparts in the
quinoline was first infiltrated into
a
pre-synthesised
aluminosilicate template (Al-SBA-15) to form hollow N-doped
carbon tubes after catalytic polymerization of quinoline with
the aid of acid sites of Al-SBA-15, followed by carbonization at
o
850 C. Then, H2PtCl6 was introduced into the hollow N-doped
State Key Laboratory of Pollution Control and Resource Reuse, Jiangsu Key
Laboratory of Vehicle Emissions Control, School of the Environment, Nanjing
University, Nanjing 210023, PR China
carbon tubes, followed by furfuryl alcohol infiltration and
o
carbonization at 850 C. Finally, the template Al-SBA-15 was
removed using a HF solution to obtain the catalysts with Pt
E-mail: srzheng@nju.edu.cn; Tel: +86-25-89680373
† Electronic Supplementary Information (ESI) available: Materials synthesis,
characterization methods, supplementary figures (Fig. S1 to S13), supplementary
table (Table S1, S2) and calculations (Calculation S1 and S2). See
DOI: 10.1039/x0xx00000x
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(calculation details presented in Calculation S1, ESI†) and the
View Article Online
results are listed in Table S1, ESI†. For Pt(0.55)/N-CMK-3,
DOI: 10.1039/C9CC05274G
uneven distribution and aggregation of Pt particles were clearly
visible (see Fig. S4(a), ESI†). Similarly, Pt(0.48)/CNT@C
presented a very broad distribution of Pt particles varying from
2 nm to 14 nm. Meanwhile, Pt/CNT wrapped by uniform carbon
shells were clearly observed in Pt(0.48)/CNT@C and Pt particles
located on the external surface of carbon shells were not
identified, reflecting that Pt particles were completely
embedded beneath carbon shells (see Fig. S4(b), ESI†). In
contrast, fine and very even distributions of Pt particles were
observed on Pt(0.39)@CMK-3 and Pt@N-CMK-3 (see Fig. S4(c)-
(g), ESI†). The average Pt particle sizes of Pt(0.48)/CNT@C and
Pt(0.55)/N-CMK-3 were calculated to be 7.54 nm and 6.46 nm,
respectively, whereas given an similar Pt loading, the average Pt
particle size of Pt(0.42)@N-CMK-3 was much smaller (2.38 nm).
The fine Pt particles and very narrow Pt particle distributions of
Pt@N-CMK-3 were likely due to the presence of N-containing
functionalities, giving rise to enhanced metal-support
interaction and Pt dispersion. Furthermore, confinement
effects from hollow tubular structure effectively suppressed Pt
particle aggregation during the carbonization process (see
Scheme 1). As for the Pt@N-CMK-3 catalysts with varied Pt
loading amounts (shown in Fig. S4(d)-(g), ESI†), the average Pt
particle sizes of Pt(0.22)@N-CMK-3, Pt(0.42)@N-CMK-3,
Pt(1.20)@N-CMK-3 and Pt(1.91)@N-CMK-3 were 1.92, 2.38,
4.56 and 5.84 nm, respectively, reflecting gradually grown Pt
particle sizes with Pt loading amount. To further evaluate the
exposed Pt particles, the chemisorption amount of CO was
measured and the results were shown in Table S1, ESI†. The
chemisorption amount of CO was 17.6 μmol g-1 for Pt(0.55)/N-
CMK-3 but below detection limit in all embedded and coated
catalysts. Correspondingly, the energy-dispersive spectroscopy
(EDS) mapping was conducted on Pt(0.55)/N-CMK-3 and
Pt(0.42)@N-CMK-3 and the images are shown in Fig. S5, ESI†.
Similar distributions of C and N elements were identified on the
catalysts, whereas the much lower density of Pt element in
Pt(0.42)@N-CMK-3 than that in Pt(0.55)/N-CMK-3 confirmed
the effective embedment of Pt in carbon rods. The results
clearly indicated that Pt particles of embedded and coated
catalysts were inaccessible for reactants.
Bromate is a carcinogenic disinfection byproduct and
reduction of bromate to bromide is an effective method to
eliminate bromate pollution in water. The liquid phase catalytic
hydrogenation reduction of bromate was used to evaluate the
catalytic performances of the catalysts. The influence of catalyst
support on catalytic bromate reduction was tested (results
presented in Fig. S6, ESI†). The control experiment showed that
bromate concentration was constant in the presence of
support, while effective bromate reduction was observed in the
presence of Pt containing catalysts, indicating that bromate was
catalytically converted. Additionally, good mass balances were
obtained on catalytic bromate reduction, reflecting that
bromide was the sole product from bromate reduction. For
catalytic bromate reduction, the initial activity calculated as the
removal rate of bromate within initial 6 min was used in order
to avoid the influence from intermediate and/or final products
on kinetic evaluation. Bromate reduction on Pt(0.42)@N-CMK-
3 with varied catalyst dosages was carried out to verify if the
reactions were conducted in the absence of mass transfer
limitation. The results showed that the initial activities
normalized by catalyst dosage were nearly constant, indicative
H2PtCl6 introduction
Infiltration
Al-SBA-15
Quinoline
Carbonization
FA infiltration and
carbonization
Template removal
Pt@N-CMK-3
Scheme1. Schematic illustration of embedment of Pt in the
carbon rods of N-doped CMK-3 using a two-step infiltration
method.
particles embedded in the carbon rods of N-doped CMK-3. In
comparison, Pt supported on N-doped CMK-3 (denoted as Pt/N-
CMK-3) was also prepared by the conventional impregnation
method.
The wide-angle and small-angle X-ray diffraction (XRD)
patterns of the samples are presented in Fig. S1, ESI†. In the
wide-angle XRD pattern of Pt(0.55)/N-CMK-3, two broad
diffraction peaks at 24o and 43o were observed, corresponding
to the (002) and (101) crystal planes of graphite structure from
porous carbon material.16 Additionally, strong diffraction peaks
at 40o and 46o were assigned to the (110) and (200) planes of Pt
particles with a face centered cubic (FCC) structure (ICDDPDF-
2#00-004-0802). For Pt(0.39)@CMK-3 and Pt(0.42)@N-CMK-3,
similar diffraction peaks corresponding to graphite structure of
porous carbon material were observed. As for Pt(0.48)/CNT@C,
strong diffraction peaks at 26o, 42o and 54o assigned to graphite
structure of CNT support were observed (see Fig. S1(a), ESI†).18
Notably, the absence of metallic Pt diffraction peaks in
Pt(0.48)/CNT@C, Pt(0.39)@CMK-3 and Pt(0.42)@N-CMK-3 was
likely due to complete embedment of Pt particles beneath
carbon matrix and/or very high Pt dispersions (small Pt particle
sizes). Small angle XRD patterns of SBA-15 template and the
catalysts are shown in Fig. S1(b), ESI†. Well resolved (100),
(110), and (200) peaks from highly ordered hexagonal
mesoporous structure were observed on the catalysts,
reflecting that the structure of SBA-15 template was perfectly
duplicated in the catalysts.17 N2 adsorption-desorption
isotherms are presented in Fig. S2, ESI† and the resulting
parameters are listed in Table S1, ESI†. The samples gave type-
IV isotherms with capillary condensation at relative pressures
(p/p0) between 0.3 and 0.8, indicative of the existence of
mesopores in the samples.19 In comparison with
Pt(0.48)/CNT@C, the catalysts with Pt particles embedded in
the carbon rods of porous carbon had much higher surface
areas and pore volumes. The surface composition of Pt(0.55)/N-
CMK-3 and Pt(0.42)@N-CMK-3 was analyzed by X-ray
photoelectron spectroscopy (XPS) and the results are compiled
in Fig. S3, ESI†. In the two catalysts, similar N 1s peaks consisting
of pyridinic, pyrrolic and graphic N species were clearly
observed. TEM images of the catalysts and the corresponding
distribution histograms of the Pt particles are presented in Fig.
S4, ESI†. The average Pt particle sizes of the catalysts were
calculated based on a surface area weighted diameter
2 | J. Name., 2012, 00, 1-3
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of the absence of mass transfer limitation under our Hinshelwood model (see Fig. S9, ESI†). The good linear
relationship
between
1/r0
andDOI: 110/.C103V9i/eCw9sAuCrtCgicg0lee5O2sn7tl4einGde
0
Fig. 1. (a) Catalytic hydrogenation reduction of bromate on
different catalysts, (b) the initial activity and normalized initial
activity with Pt loading amount. Reaction conditions: 0.1 mM
bromate, 200 ml min-1 H2 flow and 0.1 g l-1 catalyst at pH=5.6.
experimental conditions (see Fig. S7, ESI†).20
The catalytic reduction of bromate on the catalysts is
presented in Fig. 1. The initial activities of Pt(0.48)/CNT@C,
Pt(0.39)@CMK-3, Pt(0.55)/N-CMK-3, Pt(0.42)@N-CMK-3 and
commercial Pt(1.0)/C for bromate reduction were 2.1, 4.7, 11.1,
Fig. 2. The consecutive catalyst cycle of (a) Pt(0.55)/N-CMK-3, (b)
Pt(0.42)@N-CMK-3, and (c) the corresponding initial activities of
catalysts in each reaction cycle. Reaction conditions: 0.1 mM
bromate, 200 ml min-1 H2 flow and 0.1 g l-1 catalyst at pH=5.6.
10.8 and 3.7 mMgCat-1h-1, respectively, indicative of
a
decreasing order of Pt(0.55)/N-CMK-3 > Pt(0.42)@N-CMK-3 >
Pt(0.39)@CMK-3 > commercial Pt(1.0)/C > Pt(0.48)/CNT@C. It
was understandable that Pt(0.55)/N-CMK-3 exhibited the
highest activity for bromate reduction due to the presence of
exposed Pt active sites as indicated by CO chemisorption.
However, effective bromate conversion was also identified on
Pt(0.42)@N-CMK-3, Pt(0.39)@CMK-3 and Pt(0.48)/CNT@C
although Pt particles of the catalysts were completely
embedded beneath carbon overcoatings or in carbon rods. The
results clearly confirmed that H2 was capable of being activated
and bromate could be reduced on the carbonaceous
overcoatings of the catalysts with metal-carbon
heterojunctions. Additionally, Pt(0.42)@N-CMK-3 displayed a
slightly lower initial activity, but a higher Pt content normalized
activity than Pt(0.55)/N-CMK-3 (see Fig. 1(b)). Notably, the
initial activity of Pt(0.42)@N-CMK-3 was comparable or higher
than those previously reported (see Table S2, ESI†). As
carbonaceous surface acted as active sites, surface area was
likely positively correlated to the catalytic activity of the
catalyst. Notably, Pt(0.39)@CMK-3 has a specific surface area of
378.9 m2 g-1, which was 22 times higher than that
Pt(0.48)/CNT@C, while the catalytic activity of Pt(0.39)@CMK-
3 was only 2.2 times as much as that of Pt(0.48)/CNT@C,
reflecting that the catalytic activities of the embedded catalysts
were likely controlled by other factors instead of surface area of
the catalyst (see more discussion below). As compared with
that bromate reduction could be well described by Langmuir–
Hinshelwood model and the catalytic conversion of bromate
was controlled by the adsorption of bromate. Additionally,
increasing pH of bromate reduction on Pt(0.42)@N-CMK-3 led
to a monotonical decrease of initial bromate conversion,
indicative of a strong pH dependency (see Fig. S10, ESI†). Such
a strong pH dependence was ascribed to the electrostatic
interaction between bromate and the catalysts. At low pH,
anionic bromate was electrostatically adsorbed on positively
charged catalyst surface, while increasing pH led to
substantially suppressed adsorption of anionic bromate
because catalyst surface was negatively charged at high pH,
giving rise to suppressed bromate conversion.
It was notable that the catalysts with embedded metal-
carbon heterojunctions is prone to evoking Mott-Schottky
effect, resulting in electron transfer between Femi levels of
metal and CN rod.22 Accordingly, electron transfer efficiency
was strongly dependent on interfaces between metal particles
and CN rods. To evaluate the interface effects, Pt@N-CMK-3
catalysts with varied Pt loadings and Pt particle sizes were
prepared and the catalytic bromate reduction on the catalysts
is presented in Fig. S11(a), ESI†. The initial activity increased
from 6.7 to 18.0 mMgCat-1h-1 with the increase of Pt loading
from 0.22 to 1.91 wt.%, reflecting a more effective bromate
removal with the increase of Pt-CN interface. The initial
activities of the catalysts were normalized by interface areas of
Pt-CN heterojunctions assuming spherical Pt particles and close
contact between Pt particles and CN rods in the catalysts and
the results are presented in Fig. S11(b), ESI†. Despite of varied
Pt particle sizes, specific surface areas and Pt loading amounts,
the catalysts exhibited nearly constant interface area
normalized reaction rates for bromate reduction, clearly
indicative of the crucial role of interface between metallic Pt
and CN rods.
Pt(0.39)@CMK-3,
a
higher activity was observed on
Pt(0.42)@N-CMK-3, likely attributed to the presence of N-
containing functionality with a higher PZC (6.57) (see Fig. S8,
ESI†), resulting in the strong electrostatic attractive interaction
between N-doped carbon surface and anionic bromate.21 In
parallel, the much higher activity of Pt(0.55)/N-CMK-3 was
because of its higher Pt dispersion and enhanced bromate
adsorption resulting from N-doping although commercial
Pt(1.0)/C had a higher Pt loading.
To verify the role of
To test catalyst stability, the consecutive catalytic reduction
of bromate was conducted on Pt(0.55)/N-CMK-2 and
Pt(0.42)@N-CMK-3 and the results are presented in Fig. 2. After
five consecutive catalytic cycles, the initial activity of
bromate adsorption, the catalytic reduction of bromate with
varied initial concentrations (C0) was carried out on Pt(0.42)@N-
CMK-3, and the reaction data were fitted to the Langmuir–
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Pt(0.55)/N-CMK-3 rapidly decreased from 11.1 to 2.0 mMgCat-
1h-1. In parallel, ICP analysis indicated that the Pt content of
Pt(0.55)/N-CMK-3 decreased by 58.2% after five catalyst
recycles. Additionally, TEM results indicated that Pt particle size
of the used catalyst was smaller than that of fresh one (See Fig.
S12 (a) and (b), ESI†). Hence, the obvious deactivation of
Pt(0.55)/N-CMK-3 was mainly ascribed to the loss of large Pt
particles during the catalytic reaction due to weak interactions
5
6
7
G. W. Zhan and H. C. Zeng, Chem. Mater., 2015, 27V,ie7w26Ar.ticle Online
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8
between Pt particles and carbon support despite of the 9 (a) V. Bernales, D. Yang, J. Yu, G. Gümüşlü, C. Cramer, B. Gates and
presence of N-containing functionalities. In contrast, the initial
activity of used Pt@N-CMK-3 after five catalyst cycles was 10.3
mMgCat-1h-1, which was nearly identical to that of fresh catalyst
(10.8 mMgCat-1h-1), indicative of negligible catalyst deactivation
and very high catalytic stability. Furthermore, Pt contents of the
used and fresh Pt(0.42)@N-CMK-3 were measured to be 0.42
and 0.41 wt.%, respectively. In parallel, Pt particle size of used
L. Gagliardi, ACS Appl. Mater. Interfaces, 2017, 9, 33511; (b) P.
Serna and B. C. Gates, Acc. Chem. Res., 2014, 47, 2612; (c) M.
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J. Huang and M. Mavrikakis, Science, 2014, 346, 1498.
Pt(0.42)@N-CMK-3 (2.46 nm) was identical to that of fresh one 10 T. Fu, M. Wang, W. M. Cai, Y. M. Cui, F. Gao, L. M. Peng, W. Chen
(2.38 nm) (Results shown in Fig. S12 (c) and (d), ESI†). The and W. P. Ding, ACS Catal., 2014, 4, 2536.
results clearly showed that the novel structure of Pt@N-CMK-3 11 M. H. Li, J. He, Y. Q. Tang, J. Y. Sun, H. Y. Fu, Y. Q. Wan, X. L. Qu, Z.
with embedded Pt particles in carbon rods could effectively Y. Xu and S. R. Zheng, Chemosphere, 2019, 217, 742.
suppress catalyst deactivation. Accordingly, the high catalytic 12 (a) T. Chen, S. Q. Guo, J. Yang, Y. D. Xu, J. Sun, D. L. Wei, Z. X. Chen,
stability was also observed on Pt(1.91)@N-CMK-3 (Results
shown in Fig. S13, ESI†).
B. Zhao and W. P. Ding, ChemPhysChem, 2017, 18, 3454; (b) K. X.
Zhang, H. Su, H. H. Wang, J. J. Zhang, S. Y. Zhao, W. W. Lei, X. Wei,
X. H. Li and J. S. Chen, Adv. Sci., 2018, 5, 1800062.
In summary, we have fabricated a novel Pt@N-CMK-3
catalyst with fine Pt particles embedded in N-doping carbon 13 H. N. Pham, A. E. Anderson, R. L. Johnson, T. J. Schwartz, B. J.
rods using a two-step infiltration method. The fine Pt particles
as well as even Pt particle distribution are obtained as a result
O'Neill, P. Duan, K. Schmidt-Rohr, J. A. Dumesic and A. K. Datye,
ACS Catal., 2015, 5, 4546.
of the confinement effect from the ordered mesoporous 14 B. Sun, T. J. Fu, and H. C. Zeng. Chem. Commun., 2018, 54, 7030.
structure of CMK-3. N-doping and high surface area of carbon 15 (a) F. Jiao and H. Frei, Chem. Commun., 2010, 46, 2920; (b) F. Jiao
matrix provide more appropriate active sites for the adsorption
and H. Frei, Angew. Chem. Int. Ed., 2009, 48, 1841.
and reduction of bromate. Furthermore, the embedment of Pt 16 (a) X. Ji, P. S. Herle, Y. Rho and L. F. Nazar, Chem. Mater., 2007,
particles in carbon rods of N-doping CMK-3 matrix effectively
increases the interface areas between Pt and carbon rods and
19, 374; (b) Z. Wen, X. Wang, S. Mao, Z. Bo, H. Kim, S. Cui, G. Lu,
X. Feng and J. Chen, Adv. Mater., 2012, 24, 5610.
meanwhile inhibits leaching and aggregation of Pt particles. 17 (a) J. Xiao, X. Pan, S. Guo, P. Ren and X. Bao, J. Am. Chem. Soc.,
Accordingly, Pt@N-CMK-3 displays superior catalytic
performances in the liquid catalytic hydrogenation of bromate
2014, 137, 477; (b) S. Yang, X. Zhang, H. Mi, and X. Ye, J. Power
Sources, 2008, 175, 26.
to Pt/N-CMK-3, Pt@CMK-3 and Pt/CNT@C. The findings in this 18 (a) X. K. Li, W. J. Ji, J. Zhao, S. J. Wang and C. T. Au, J. Catal., 2005,
work demonstrate that embedding metal particles in porous
carbon matrix provides a new avenue to effectively utilize noble
metals in heterogeneous catalysis.
236,181; (b) L. Borchardt, E. Kockrick, P. Wollmann, S. Kaskel, M.
M. Guron, L. G. Sneddon and D. Geiger, Chem. Mater., 2010, 22,
4660.
This work was supported by the National Natural Science 19 (a) D. Zhao, J. Feng, Q. Huo, N. Melosh, G. H. Fredrickson, B. F.
Foundation of China (No. 21577056) and Outstanding Youth
Foundation of Jiangsu Province of China (No. BK20190301).
Chmelka and G. D. Stucky, Science, 1998, 279, 548; (b) S. Jun, S.
H. Joo, R. Ryoo, M. Kruk, M. Jaroniec, Z. Liu, T. Ohsuna and O.
Terasaki, J. Am. Chem. Soc., 2000, 122, 10712.
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O. M. Ilinitch, F. P. Cuperus, L. V. Nosova and E. N. Gribov, Catal.
Today, 2000, 56, 137.
Conflicts of interest
21 (a) G. P. Mane, S. N. Talapaneni, C. Anand, S. Varghese, H. Lwai,
Q. M. Ji, K. Ariga and T. Mori, A. Vinu, Adv. Funct. Mater., 2012.
22, 3596; (b) P. Zhang, F. Jiang and H. Chen, Chem. Eng. J., 2013,
234, 195.
There are no conflicts to declare.
22 (a) X. H. Li and M. Antonietti, Chem. Soc. Rev., 2013, 42, 6593;
(b) Y. Zhou, K. Neyerlin, T. S. Olson, S. Pylypenko, J. Bult, H. N.
Dinh, T. Gennett, Z. Shao and R. O’ Hayre, Energy Environ. Sci.,
2010, 3, 1437.
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