ordered mesoporous carbon and its applications for
TRANSCRIPT
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Ordered Mesoporous Carbon and Its Applications for Electrochemical Energy Storage and
Conversion
Ali Eftekhari a,b,*, Zhaoyang Fan c,*
a The Engineering Research Institute, Ulster University, Newtownabbey BT37 OQB, United
Kingdom
b School of Chemistry and Chemical Engineering, Queen's University Belfast, Stranmillis Road,
Belfast BT7 1NN, United Kingdom
c Department of Electrical & Computer Engineering and Nano Tech Center, Texas Tech University,
Lubbock, Texas 79409, USA
Abstract
Ordered mesoporous carbon (OMC) is a flexible material providing interconnected channels for the
diffusion of electroactive species in electrochemical systems. This is a unique feature, which
distinguishes OMC from other types of carbonaceous materials including mesoporous carbon (MC).
The potentials of OMC in electrochemical systems have been overshadowed by the vague
terminology of this class of mesoporous materials. Despite the ordered structure of mesopores, the
electrochemistry of OMC is not straightforward. This manuscript reviews the opportunities
experimentally presented for employing OMC in various electrochemical power sources such as
ultracapacitors, supercapacitors, battery systems, fuel cells, and electrochemical hydrogen storage.
The aim is to highlight the potentials and critical issues. For instance, the graphitization of OMC is
of particular importance, as ordered alignment of π electrons can be beneficial for charge transfer;
while the mesopore edges can resemble the peculiar properties of graphene edges.
Keywords: Ordered mesoporous carbon; supercapacitor, lithium-ion battery, lithium-air battery,
lithium-sulfur battery, fuel cell
Email: [email protected]; Email: [email protected]
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1. Introduction
Owing to its unique flexibility in forming nanostructures, carbon has found a central role in the
realm of nanotechnology, with fullerenes, carbon nanotubes, and graphene as the landmark
discoveries [1]. A new member of this family is ordered mesoporous carbon (OMC), which has
recently attracted considerable attention.
On the other hand, porous carbon materials, although not so exciting, has a much longer practical
application history. With their remarkable physicochemical properties, including large specific
surface area (SSA) and pore volume, high corrosion resistance, good thermal and mechanical
stability, and further considering their easy manufacturing and precursor earth abundance, porous
carbon has been employed in various applications. These include water and air filtration, as
catalysts or catalyst supports, gas storage host, and electrochemical energy storage and conversion.
It is still a dominant characteristic material for such applications.
According to the IUPAC classification of porosity, micropores are < 2 nm, mesopores 2–50 nm,
and macropores > 50 nm. Traditional porous carbon materials, including activated carbons and
carbon molecular sieves, are commonly synthesized in a pyrolysis process with appropriate carbon
precursors such as coal, polymers, and carbides, with the activation through potassium hydroxide [2]
or selective etching of metal ions in carbides by halogen gasses [3]. Associated with these
micropore-dominated carbon materials are drawbacks that include slow mass transport in the
micropores, low electrical conductivity resulted from abundant surface groups and defects, and
porous structure collapse at high-temperature, among others.
From the consideration of molecules diffusion and electrolyte ions transportation, mesoporous
carbon (MC), those dominated with 2-50 nm mesopores, are more interesting, since microspores
might not be easily accessible by these species, while macropores are simply too large leading to a
reduced SSA. Therefore, MC was subsequently developed through a variety of strategies [4-9].
These MC materials have a broad pore-size distribution without structural ordering (or symmetry).
Indeed, MC is a general category according to the physical porosity and does not necessarily
represent the same geometrical structure. Mesoporosity of carbon in the form of nanostructured
texture obviously increases the specific surface area. Of course, the disordered pores are
unpredictable in electrochemical performance, as the pores are not necessarily electrochemically
accessible.
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OMC certainly can be regarded as a natural evolution from MC when constraints of narrow pore
size distribution with ordered pore positions are applied. Strictly speaking, if a perfect ordering is
defined for a specific pore size on a macro-scale, such OMC will belong to the category of
superlattice or meta-materials with unique properties due to its 2D or 3D periodical structure
resulting in quantization of wave vectors (i.e., dramatically different from MC with random pore
size and random pore position). However, from a practical point of view in electrochemistry,
neither a perfect pore ordering nor the same pore size is necessary. OMC, with either a non-perfect
ordering or a non-uniform pore size, due to the easier fabrication and control, is under active
investigation for much better performance in many applications that traditionally employ MC or
porous carbon. This is particularly true for electrochemical energy conversion and storage. The
explosive increase in the number of papers published in the very recent few years witnesses the
research interest in this field.
In this review, we will first summarize the synthesis methods and novel OMC properties, and then
focus on its applications for electrochemical energy conversion and storage, including
supercapacitors, lithium-ion batteries (LIB), other emerging rechargeable batteries, and others.
2. Ordered Mesoporous Carbon: Synthesis and Properties
2.1. From Mesoporous Carbon to Ordered Mesoporous Carbon
Mesoporous carbons could be synthesized by different methods, such as catalytic activation of
carbon precursor using metal-containing species [9-10], carbonization the blends of one
thermosetting precursor and one thermally unstable polymer [7], and carbonization of organic
aerogels [11]. The produced mesopores from these methods generally have a broad size distribution.
They also introduce a lot of micropores. Well-controlled pore size distribution through template
method, therefore, became more interesting.
The story started by attempts for utilizing silica gel as the template for the preparation of
carbonaceous materials. In the 1980s, synthesis of MC was investigated by impregnating phenol-
hexamine mixture as carbon precursor into silica gel as a template [12]. Owing to the spacious
structure of silica gel, carbon precursor can be easily inserted. Upon completing the carbonization
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process, the silica template then can be easily removed. Although the resulted MC has no structural
ordering (symmetry), this effort provided the strategy of template-guided OMC synthesis, as long
as an ordered template with suitable dimensions is available. Liquid crystals provide an ordered
structure with the mobility of liquid, which can be used as mesoporous templates. This feature was
utilized in 1992 to fabricate mesoporous molecular sieves [13-14] and led to the birth of an
interesting family of ordered mesoporous materials with crystal-like symmetries. Carbon is usually
a pioneer in forming new nanostructures, but cannot be synthesized chemically in liquid through the
liquid crystal template. Hence, OMC is synthesized by utilizing the mesoporous silica templates
originally prepared by the liquid crystal template [15-17]. For about two decades started in the
1980s [12,18-19], various silica and zeolite templates were utilized for the preparation of MC. The
birth of OMC did not happen until 1999 when cubic mesoporous aluminosilicate MCM-48 was
employed as the hard template [15,20], thus creating a new nanocarbon structure with symmetry.
Currently, OMC that has a very narrow pore-size distribution with periodical structural ordering are
synthesized using a template. Depending on the template used, the OMC synthesis can be
differentiated into two categories: hard-templating based (impregnation and etching back) and soft-
templating based (direct synthesis). Their major differences are illustrated in Figure 1.
Figure 1. Schematic comparing a) hard-template based and b) soft-template based synthesis
strategies. Reproduced with permission from Ref.[19]. Copyright 2006, Wiley-VCH.
2.2. OMC Synthesis: Hard-Template Based
In this strategy, an order mesoporous solid template is applied as the mold for the negative
replication of OMCs. The pore size control and symmetric ordering are simply determined by the
solid template and do not rely on the interaction between the carbon precursor and the template.
The development of hard-template based OMCs was comprehensively reviewed by Dai et al. [4]. In
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this hard-templating synthesis strategy [19], a preformed hard template, particularly that silica
based ordered mesoporous structures are used, and carbon precursors are impregnated into the pore
volume. After carbonization, the hard template is etched away, leaving the negatively replicated
OMC. That is, the interconnected pore space in the template is transferred into the continuous
framework of OMC, while the volume once occupied by the template material becomes mesopores
in OMCs. 3D interconnected porous structure of the template is generally considered to be
necessary for this process. The success of using SBA-15 silica mesoporous molecular sieve as a
template, which has a cylindrical pore structure, is due to the existence of interconnecting
micropores in the sidewalls. It is worth mentioning that, in addition to the solution-based
impregnation to fill the precursor into the pore volume of the template, chemical vapor deposition
was also capable of filling the pore volume.
Template candidates: Silica-based order mesoporous structures such as MCM, SBA, FDU, MSU-H,
and HMS series have contributed to the synthesis of a variety of the OMC structures such as cubic
structures with several symmetries, face-centered cubic, body-centered cubic, and 2D hexagonal
structure. There are also some efforts focusing on the use of as-synthesized ordered structures of
colloid nanoparticles (NP) as the hard templates. The OMC pore size now is primarily determined
by the NP size, and therefore, the pore size can be easily adjusted in a large range [21]. Silica NPs,
polymer beads such as polystyrene spheres and others can be used. Iron oxide NPs are interesting
[22] since iron can catalytically induce graphitization at lower temperatures (< 1000 °C) [23].
The key advantage of silica-based templates is the highly ordered architecture of the mesopores, but
a key disadvantage is the essential requirement of acid treatment for the template removal. The
strong acid treatment does affect the carbon surface and its functionality. Although the defects
formed might be useful in the electrochemical system, the material ordered architecture is lost at the
atomic scale. Other templates such as MgO has also been introduced [24-26], which can be
removed with a light acid treatment, but the uniformity of the mesopores is not at the level of silica-
based templates. However, another considerable advantage of such templates is a practical
feasibility for scaling up the material production.
Carbon precursors: During the high-temperature carbonization and graphitization process, the
molecular structure of the precursor will determine the shrinkage of the structural frame and the
possibility of micropore generation in the frame, and therefore, the morphology and SSA of the
OMC formed. Commonly applied precursors can be categorized into those with loose molecular
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structures such as sugar, sucrose and furfuryl alcohol, and those with dense aromatic structures such
as pitch, pyrene, polyacrylonitrile, and acenaphthene. Using the latter category of precursors, the
OMC could replicate the reverse image of the hard templates with minimum framework shrinkage,
high mechanical strength, and negligible microporosity. In contrast, if precursors with loose
structure are applied, framework shrinkage will increase the mesopore size, and particularly
micropores will be generated in the framework, leading to bimodal pore-size distribution and larger
SSA. When an SBA-15 silica template is used, micropores in the OMC can also be produced due to
the micropores in the pore walls of the template [27-28].
Although silica is an ideal template for the preparation of OMC, template removal is time-
consuming and somehow destructive to achieve complete removal of silica. Other mesoporous
templates can have some advantages. For instance, electroactive materials are excellent templates if
the target application of OMC is in electrochemical systems. For instance, mesoporous nickel oxide,
which is an electroactive material for supercapacitors, have been successfully utilized to prepare
OMC [29].
With the sacrifice of the template used, this hard-template based strategy has its intrinsic limitation
on cost. However, it does have several prominent advantages. The impregnation mechanism offers
a relatively facile process to precisely replicate the negative image of the hard template, and the
nature of the hard template ensures the pyrolysis process causing less damage on the structure
regularity and ordering. Another prominent merit of this method is easier graphitization of the
OMC formed within the hard template.
2.3. OMC Synthesis: Soft-Template Based
Instead of sacrificing the template by etching it away, it is possible to directly synthesize OMC by
self-assembling a block copolymer surfactant and carbon precursor [4,30-34]. The advantage of this
method is the absence of template removal step, which is somewhat destructive. The OMC with
mesopores in the range of 3–7 nm can be easily synthesized by this method. The interaction
between the carbon precursor and the surfactant, which drives the self-assembly of the soft template,
determines the pore structure. This strategy is rooted in the pioneering work on the M41S family
silica materials [13]. The association of surfactant micelles with the precursor through a weak
interaction, such as hydrogen bonds, leads to the polycondensation of the precursor. The self-
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assembly of the composite micelles yields an ordered mesostructured. The removal of the soft
template and further carbonization of the remaining precursor polymer yields the OMC with a
defined symmetry and pore size.
Since the early report of the soft-templated OMCs by a stepwise assembly approach [30], great
progress has been made to synthesize OMCs using this method, as has been comprehensively
reviewed by the Yuan’s group [35]. A variety of OMCs were synthesized in the forms of spheres
[36], rhomb dodecahedron [37], wires [38] and ribbons [39], films [30], or monoliths [40]. The
strategy, through the supramolecular assembly of the soft surfactant templates, can be accomplished
by an evaporation-induced self-assembly (EISA) or hydrothermal process. The EISA of a block
copolymer and resols is a facile approach with flexibility since it can separate the cross-linking and
thermo-polymerization process of the resols from the self-assembling process. The ordered
mesostructure is formed on the solvent evaporating surface, and therefore, the OMC films could be
produced. Different OMCs with 2D hexagonal, lamellar, 3D bicontinuous, body-centered cubic,
and other structures have been prepared using this route [41]. Using water to replace the organic
solvents is an alternation [42], in which the surfactant-driven self-assembly and carbon precursor
polymerization occur in a cooperative process. Such an aqueous route offers better reproducibility
and suitable for large scale production. The hydrothermal process was also reported to fabricate
OMCs [36,40].
Direct synthesis with surfactant recycling provides the opportunity for a large-scale production. The
challenge of this strategy is that currently available options of the soft templates is mainly limited to
block copolymers and the precursor to phenolic resin. The block copolymer limits the minimum
pore size to ca. 3 nm. Smaller amphiphilic molecules as templates should be explored for smaller
pore size.
Comparing the OMCs synthesized from these two strategies, the soft-template OMCs have thick
pore walls with a continuous framework, thus, offer stability in harsh thermal and oxidation
treatment for functionalization. However, the hard-template OMCs is much easier to be graphitized,
while it is difficult for the soft-template OMCs.
The morphology of the OMCs (including specific surface area, pore size, and volume) can be
altered by post-synthesis modification. KOH activation is a common method industrially employed
for generating the micropores in activated carbon [2,43-45]. Depending on the activation conditions
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(temperature, concentration, etc.), micropores generated can merge into each other to form
mesopores or create microporosity texture. In the latter case, micropores can build shortcut bridges
between mesopores, which can be beneficial for electrochemical performance [46]. This method of
activation can double the specific surface area of OMC.
2.4. Graphitization of OMC
It is sometimes wrongfully addressed that OMC is not a graphitic material. Considering the fact that
amorphous carbon is actually a form of disordered graphite, these types of carbonaceous materials
are always graphitic with different degrees of graphitization, which is usually judged by the D and
G bands in Raman spectroscopy. From a practical perspective, the OMCs with higher graphitization
degree are better for various applications. This is particularly true for the electrocatalyst and
electrode applications in which higher electrical conductivity critically depends on the degree of
graphitization [47]. Thus, there is a demand for increasing the degree of graphitization of the OMCs.
Low-temperature carbonization offers well-ordered structure, but with an amorphous or low degree
of graphitization framework. Post-synthesis thermal treatment [48], particularly if conducted at a
high temperature (> 2000 °C) will induce significant graphitization, but resulting in a lower degree
of ordering with broad pore-size distribution. Carbon precursors with rich fused aromatic structures
such as polyaromatic hydrocarbons or aromatic molecules [23,49-54] are better than those with
loose molecular structures since the former can be graphitized at much lower temperatures,
particularly when the iron-based catalyst is incorporated [27,55]. CVD growth at a temperature
higher than 900 °C is another option [56], leading to the formation of graphitic OMCs [56-59]. In
almost all methods, the reaction or treatment is conducted at a high temperature where carbon
atoms have enough energy to arrange or re-arrange themselves into the graphitic hexagonal form
[60]. The temperature could be lowered in the presence of catalytic species, particularly iron-based
nanomaterials.
A simple and effective approach is carbonization of metal phthalocyanines within an SBA-15
template [59]. However, this method is not practical because of the high cost of phthalocyanines. It
has been reported that phthalocyanine can be replaced by natural fat as the carbon feedstock in the
same template system to produce the OMCs with graphitic walls at relatively low temperature [61].
A new approach is to utilize a triblock-copolymer template, which results in the formation of highly
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graphitic OMCs while the mesopore size is strongly tunable in the range of ca. 3 – 40 nm [30-
31,62-63].
Graphitization of OMC is of particular importance in electrochemical systems, as increases the
electrical conductivity, which is indeed a major requirement to reduce the charge transfer resistance.
In the lack of appropriate graphitic conductivity, the electrical conductivity of OMC should be
improved by some conductive agents such as graphene or metals to achieve required conductivity
for electrochemical performance [64-73].
2.5. OMC with Graphene Wall
Graphene foam has been developed in the recent studies of graphene-based electrode applications.
Chemically-derived individual reduced graphene oxide sheets, with a sub-micrometer size, can be
assembled into a foam structure through freeze-drying or similar methods [74-76]. Such a graphene
foam has irregular pore distribution, and particularly, they do not form an intimately connected
network. Direct growth of multilayered graphene (MLG) inside of a 3D metal frame resulted in
macro-pores of a few hundred micrometers in diameter by the metal foam template [77]. Both are
not the optimized electrode structures when compared to the graphitized OMC structure with
graphene wall.
The OMC with graphene wall is a variation of graphitized OMC when the highly graphitized pore
wall is thinned down to a few atomic layers. The soft-template based method will not provide the
high degree of graphitization and therefore unsuitable for producing the graphitized OMC; while
for the hard templates, in order to obtain pore walls of graphitized OMC down to several atomic
layers, the void space in the hard templates should be thin enough. Furthermore, the high degree of
pore ordering and graphitization demand a catalytic graphitization process at a moderate
temperature.
Jang et al. [78] reported the growth of mesoporous graphene balls (MGBs) using a drop-casted
polystyrene bead (PS) as a template. As illustrated in Figure 2a, carboxylated PS was synthesized
via emulsion polymerization and then sulfurized to obtain SPS-COOH, which can strongly absorb
iron ions (Fe3+) when emerged in the FeCl3 solution. Using the drop-casted beads as a template and
precursor, the sample was annealed in H2/Ar environment to catalytically promote the graphene ball
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growth. Thus, the resulting graphene balls have a diameter similar to that of the functionalized PS
beads, but etching away the Fe from the sphere walls will form the MGBs, as shown by the
transmission electron microscopic (TEM) images in Figure 2b,c. Due to the irregular distribution of
the PS beads in the template, the synthesized MGBs did not form an ordered 3D macrostructure.
Figure 2. a) Schematic of MGB synthesis from drop-casting functionalized beads/FeCl3 solution, to
thermal annealing for graphene growth, and etching away Fe domain to obtain MGB. b,c) TEM
images of MGB. Reproduced with permission from Ref.[78]. Copyright 2013, American Chemical
Society.
Dong et al.[22,79] took one step further to synthesize the graphene OMCs with superlattice
symmetry. In their works, the Fe3O4 colloidal NPs formed a superlattice structure, which was
employed as both template and catalyst. Using oleic acid (OA) capped Fe3O4 colloidal nanocrystals
(NC), a 3D superlattice was self-assembled and followed by the carbonization/graphitization of the
OA ligands at 500 °C in the presence of an iron catalyst. The partially-graphitized OMC after the
NC removal is shown in Figure 3a,b. Further heat treatment at 1000°C results in the formation of
multilayered graphene as pore wall (Figure 3c,d). The resulting graphitized OMC exhibits a long-
range highly-ordered superlattice symmetry, replicated from the template.
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Figure 3. a) Schematic of the OMG synthesis from colloidal Fe3O4 NPs. b,c) TEM images of the as-
synthesized OMC superlattice after catalytic carbonization at 500 oC with fcc symmetry. d,e) TEM
images of OMG after further graphitized at 1000 oC, imaged for (111) plane. Reproduced with
permission from Ref.[22]. Copyright 2015, Wiley-VCH.
Huang’s group [80] employed SBA-15 as a template and poly furfuryl alcohol (PFA) as a precursor
to synthesize a graphitized OMC. Figure 4 demonstrates the synthesis procedure. First, an
impregnated template if formed by depositing the Ni agent within the silica template, then the N-
doped ordered mesoporous with walls made of few-layer carbon are built within the template in a
CVD process. The final step is the removal of the template and the metallic catalyst.
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Figure 4. a) Schematic to synthesize nitrogen doped OMG. b) Low-angle x-ray diffraction patterns
of the synthesized sample with or without N-doping, showing the characteristic peaks of hexagonal
packing. Reproduced with permission from Ref.[80]. Copyright 2015, American Association for the
Advancement of Science.
2.6. Graphene Edge-Oriented Pore Walls
For these highly graphitized OMCs, the graphite basal plane is generally exposed as the pore wall
surface. In electrochemical systems, the graphite basal plane is far less attractive than the edges.
Ideal graphene is not an interesting material in term of electrochemical reactions due to the high
ratio of the basal plan to edges, and particularly flatness of the hexagonal network of carbon atoms
in which the sp2 hybrid is not very reactive [81]. The later is somehow shielded by the π electrons
avoiding direct adsorption at carbon atoms. It is known that the edge plane of highly oriented
pyrolytic graphite has an electrochemical reactivity several orders of magnitude higher than its
basal plane due to a large amount of defects, such as kinks, steps, and vacancies, at the edge that
produce a high density of defect states near the Fermi level [82]. These atomic edges or steps are
the potential adsorption sites of redox species in the electrolyte and sites of electron transfer. The
edge planes can also provide electrical double layer capacitance of 50 to 70 mF cm-2 in comparison
with that of basal planes, which provide a capacitance of only ~3 mF cm-2 [83]. The edge-oriented
multilayered graphene flakes have been investigated for a variety of electrochemical applications
[84-87]. Therefore, it is highly desirable to synthesize the OMCs with exposed graphene edges.
Using Al-incorporated silica templates and various aromatic compounds as a precursor in an
autoclave process, followed by further graphitization at high temperatures, Ryoo's group [55]
demonstrated a unique CMK-3 OMC with graphitic framework structures through in situ
conversion of the aromatic compounds to mesophase pitch inside the silica templates. The degree of
graphitization of OMC can be at the level of multi-walled carbon nanotubes or multiple-layer
graphene. A striking feature is that the hexagonal arrays of carbon nanorods are formed by a
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stacking of the discoid graphene sheets oriented perpendicular to the rod orientation, with the
exposed edge-on graphitic structure, as shown in Figure 5.
Figure 5. a) Schematic of CMK-3G OMG consisting of hexagonal arrays of carbon nanorods, while
the nanorods is formed by a stacking of the discoid graphene sheets oriented perpendicular to the rod
orientation. b) TEM images of CMK-3G showing the rod array. c) TEM images showing the stacked
discoid graphene sheets. The inset is the corresponding electron diffraction pattern. Reproduced with
permission from Ref.[83]. Copyright 1971, The Electrochemical Society.
Utilizing nickel foam [88] or cellulose paper [89] as a template, Ren et al. deposited edge-oriented
multiple-layer graphene porous structure in a plasma CVD process and the template can be
removed [90]. Since the template used has large pores without ordering, the edge-oriented graphene
porous structure thus produced does not belong to the category of graphitized OMC. However, if
suitable templates are used, such a plasma CVD process may provide a viable approach for
producing edge-oriented graphitized OMC.
In general, there are various methods to enhance the degree of graphitization of the OMCs to align
the π electrons along the ordered architecture, and it is still an active area of research. However, our
knowledge about the arrangement of graphene hexagons across the mesopores is very limited. In
the graphene structure, edge atoms have anomalous electronic properties resulting in different
electrochemical performance. However, the actual atomic structure of the edges of OMC mesopores
is not fully understood.
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3. OMC in Electrochemical Systems
3.1. Electrochemistry of OMC
A comparative study revealed that the electrochemical activity of the OMC is higher than that of
graphene, which is a popular material in the realm of electrochemistry [91]. In a sense, the OMC is
considered as an alternative to the classical microporous carbon materials which have been
commercially available for decades. Therefore, the goal of the OMC production is to achieve the
highest possible specific surface area, but this is not the main requirement in the electrochemical
systems. Microporous carbonaceous materials have an extremely high specific surface area, but
micropores are too small for the diffusion of electroactive species. Since mesopores well fit with the
size of diffusing species, the OMC has attracted considerable attention in the realm of
electrochemistry. However, the common standpoint was to employ the OMC as a high surface area
carbon. This is the reason that the majority of electrochemical studies of the OMC are focused on
supercapacitors [92-104] or sensors [105].
The characteristic feature of the OMC in electrochemical systems is the possibility of fast diffusion
through the solid electroactive material. Unfortunately, our understanding of the electrochemistry of
OMC is very limited, as fewer efforts have been paid to this important issue. There is a similar
situation about electrochemistry of graphene because graphene is not as simple as the flat hexagonal
network of carbon atoms imagined [106-108]. Instead, graphene is full of chemical and physical
irregularities which can substantially change the electrochemical process. This misleading comes
from the straightforward structure of ideal graphene, but OMC chemical irregularities are too
complicated even for an ideal structure.
The arrangement of carbon atoms at the mesopore edges is indeed a mystery, particularly as the
graphitization level of OMC is not absolute or uniform. Similar to graphene, electrochemistry at the
mesopore edges is completely different from that on internal walls of mesopores. A key difference
is that edges and dangling atoms in graphene are chemically preferred sites; but in OMC, the
mesopore edges are even physically preferred to initiate the electrochemical reactions, as they are
more accessible.
Since carbonaceous nanomaterials are subject to chemical treatment resulting in severe structural
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changes, their electrochemistry cannot be easily judged. For instance, it was claimed that a majority
of electrochemical activity of graphene samples are due to the defects formed during the post-
treatment rather than the original graphene structure [109-110]. This phenomenon is more
complicated for OMC, as the template removal is at the atomic scale. In other words, not only the
chemical treatment but also the carbon template interactions can result in peculiar defects.
Electrochemistry within the OMC matrix is probably different from that on other carbonaceous
nanomaterials and far from fully understood. For instance, double layer capacitance is a
straightforward phenomenon with least electrochemical complexity, but the specific capacitance of
OMC within its silica template is similar to that after template removal [111].
3.2. Micropores within Macroporous Structure
Internal accessibility of mesopores is not the only factor in electrochemical performance, as
electroactive species should reach the mesopores regularly. Since the rate-determining step in most
electrochemical systems is the diffusion process, it is vitally important to facilitate a fast diffusion
of electroactive species to keep them ready for the insertion into the mesopores. Note that the
charge transfer resistance for a conductive carbon with a high specific surface area is not normally
the rate-determining step. This macrostructure of mesoporous carbon is of particular importance for
the electrochemical systems. Ordered hierarchical mesoporous/macroporous carbon display good
performance in electrochemical systems, as the ordered macropores facilitate fast diffusion through
the electrolyte to mesopores [112]. Figure 6 shows the ordered structure at two different scales of
such carbonaceous materials.
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Figure 6. SEM and TEM images of the Ordered hierarchical mesoporous/macroporous carbon at
different scales. Reproduced with permission from Ref.[112]. Copyright 2013, Wiley-VCH.
Figure 7 displays how a macroporous structure can be created by mesoporous building blocks. Such
two-level porous carbon has been prepared with different methods [113]. A simple idea is to use
two different templates for the formation of macropores and mesopores simultaneously. For
instance, polystyrene is known as a good template for the formation of macropores; introducing
silica nanoparticles creates mesopores throughout the walls of macroporous carbon synthesized
[114].
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Figure 7. An illustration for designing carbon-supported Pt electrocatalyst with
macroporous/mesoporous architecture. Reproduced with permission from Ref.[113]. Copyright 2015,
Wiley-VCH.
3.3. OMC Nanocomposites
As described above, OMC is prepared to utilize mesoporous templates, which should be removed.
Depending on the properties of the template, the final material can be OMC/silica, which is indeed
a nanocomposite with potential applications. In a similar fashion, OMC can be used as the template
for the synthesis of mesoporous electroactive material; then, it is not necessary to remove the
template, as the OMC template is indeed an important component of targeted nanocomposite. This
leads to the formation of a uniformly distributed nanocomposite, which is indeed a key goal for
electroactive nanocomposites in which carbon should contribute to the electrical conductivity and
fairly separating electroactive materials to become more electrochemically accessible. OMC has
been widely used as the nanocomposite component for various electroactive materials [115].
Since the size of mesopores is too small for conducting uniform reaction therein, it is a serious
challenge to uniformly fill the mesopores with the second component. For instance, sonochemical
synthesis can result in a more uniform distribution of reactants to form the electroactive material
uniformly distributed over the OMC pores [115].
A common issue for electroactive materials is the necessity of binders to form a solid electrode.
Binders are usually electrochemically inactive and may block the diffusion of electroactive species;
besides the fact that their mass reduces the specific energy and power of electrochemical power
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sources. In addition to the possible chemical interaction of OMC with electroactive materials, the
interconnected architecture of OMC provides a rare opportunity for in situ preparation of
nanocomposites in which the electroactive material is entangled through the OMC scaffold [116-
117].
While OMC mesopores can serve as local tubes for the formation of an electroactive material,
micropores are too small and will be blocked by the resulting material for electrochemical
performance [118]. This blockage is not necessarily physical filling, as mesopores are also filled
with the electroactive material, but its lattice network is still large enough to allow solid-state
diffusion. This feature is not limited to OMC, and 3D MCs with larger mesopores are indeed good
matrix for the formation of electroactive materials [119].
4. OMC in Electrochemical Energy Storage
4.1. OMC for Ultracapacitors (Double Layer Capacitors)
High surface area carbon has always been the first choice for double layer capacitors (aka
ultracapacitors). It is not difficult to prepare a carbon with an extremely high surface area, but not
all the surface area is electrochemically accessible. Thus, most carbon-based ultracapacitors have
specific capacitance below their theoretical capacities. OMC can provide an ordered matrix for the
interfacial interaction with charged ions within the electrolyte solution. However, the limitation is
the size of mesopores. If they are too small, ions cannot freely diffuse therein, and if too large, the
specific surface area is low. In fact, the mesopores should be tuned for a specific ultracapacitor
depending on the size, charge, and structure of the electroactive species forming the double layer
[120]. Gogotsi and Simon have elaborated that dependency of specific capacitance of OMC on pore
size [121]. In general, OMC with sufficiently large pores has a specific surface area around 1,000
m2/g, resulting in specific capacitance comparable with other types of carbon [64,122-123].
However, the capacitive behavior of OMC is not straightforward as the nature of double layer
within the mesopores is still ambiguous. Different values have been reported for the specific
capacitance of similar OMCs. It has been explained that the synthesis conditions and post-treatment
have huge impacts on the electrochemical performance of OMC [124].
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Highly ordered single crystals of mesoporous carbon show excellent electrochemical performance
for ultracapacitors [125]. The large crystalline particles dictate that the electrochemical process is
conducted through the particle matrix rather than the external interface (Figure 8). Although it is not
entirely a solid-state system because electrolytes are soaked within the mesopores, the
electrochemical performance relies on diffusion through interconnected pores. This clearly indicates
that internal mesopores are responsible for the high specific capacitance achieved (281 F g–1 at 0.5
A g–1 in a 6 M KOH electrolyte) rather than having high surface area because of smaller particles.
The importance of this feature is because of the essential requirement of the electroactive packing
within the electrode structure. It seems that larger particles, which are of practical interest, with
mesoporosity, can provide a large electrochemically accessible area. However, it should be taken
into account that the cyclic voltammetric behavior indicates that the system is not purely capacitive.
In addition to the complicated pseudocapacitive contribution, the solid-state diffusion is a rate-
determining step when the electrochemically accessible area is mostly spread through the internal
mesoporosity.
Figure 8. (a-h) SEM and TEM images of an N-doped OMC with Im3m symmetry and rhombic
dodecahedral single crystal morphology. (i) Cyclic voltammograms and (j) charge/discharge profiles
of the N-doped OMC as an ultracapacitor. Reproduced with permission from Ref.[125]. Copyright
2015, Royal Society of Chemistry.
The best capacitive behavior of OMC is obtained when the degree of graphitization is maximum
[126-127]. Since graphene basal plane is not electrochemically active [109-110], the formation of
graphitic walls along the 001 direction assists charge transfer between the electrode/electrolyte
interface and the current collector. Furthermore, the shape and structure of the double layer over the
basal plane of graphene is different from those on amorphous walls of mesopores.
The unique feature of OMC is its translational symmetry of its unit cell, but the internal structure of
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the unit cell of mesopores can have a rough texture. Although micropores are too small for long
diffusion of electroactive species, the presence of microporous texture on the walls of mesopores
can be beneficial for ultracapacitor performance as far as they are accessible [128-129].
Highly ordered nanofibers of OMC provide an architecture for more effective diffusion of the
electroactive species across the electrode matrix. OMC nanofibers display a well-defined capacitive
behavior [130]. On the other hand, as the nanofibers can be prepared by an AAO hard template, it is
possible to directly grow them on the current collector, which is in favor of the overall electrical
conductivity and suitable for high-power micro-supercapacitors [131]. The hollow structure can
provide a better accessibility of the mesopores from both sides, and the specific capacitance of a
fibrous-structured hollow OMC has been reported to be very high (359 F g–1), and particularly an
extremely large power density (10 kW kg–1) in a 6 M KOH electrolyte [132].
In a similar fashion, OMC can be directly synthesized on a polymer substrate to form a flexible film
[133]. It is a general demand to make the electrochemical cells flexible for wearable electronics,
which is realistic by the development of gel electrolytes; however, electrode materials are usually
fragile, and the main obstacle still exists in this direction.
The superiority of OMC for supercapacitors is not limited to its high surface area. It is well known
that purely double layer capacitor based on the carbonaceous material is not realistic, as there are
always some faradaic redox reactions. This is preliminary because of the functional groups formed
or adsorbed on the active surface of the carbon. This behavior is more studied for the functional
groups on graphene, particularly chemically-derived reduced graphene oxide [134-136], but similar
mechanisms are also applied to surface-modified OMC. The presence of various functional groups
can significantly alter the electrochemical performance of OMC [137]. Chemical treatment or
activation of OMC results in the formation of such functional groups, which are responsible for part
of the superior ultracapacitor performance [138].
Similarly, graphene edges play particular roles in electrochemical systems, as the charge transfer
mechanism and barrier can be utterly changed through the dangling bonds at kinks, steps, and
vacancies at the edge that produce a high density of defect states near the Fermi level [139].
Therefore, the graphite edge plane offers a capacitance 20 times larger than the basal plane. This
feature can also be the case for OMC pores having sharp edges. Nevertheless, the structural
arrangement of carbon atoms in OMC has not been fully understood yet. The peculiar charge
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transfer can be controlled by the morphological structure or degree of graphitization of OMC.
Similar to the role of functional groups, doping alters the uniformity of charge distribution across
carbon atoms, and chemical reactivity to have more contributions of pseudocapacitive nature.
Nitrogen is the most common element for doping of various types of carbon, which also enhance
their electrical conductivity. It has also been widely used for the doping of OMC [140-149]. Owing
to the pseudocapacitive contribution, the specific capacitance of N-doped OMC is over 300 F g–1 in
a 1 M H2SO4 electrolyte [150].
Another important feature of doping is to enhance the wettability of OMC, which is a serious
requirement for ultracapacitors, and also other electrochemical applications. Pristine OMCs
normally have hydrophobic nature, and thus, poorly forming the electrode/electrolyte interface. N-
doping can scientifically contribute to the surface polarity of OMC, but it is not easy to dope a high
content of nitrogen. The presence of a Pluronic surfactant having a high content of oxygen in the
OMC synthesis interact with N-rich carbon precursor to decompose it. This results in deformed
mesostructure, and thus, N-doping sacrifices the uniformity and order of OMC [151-153]. On the
other hand, simply increasing the amount of nitrogen dopant is not beneficial for the ultracapacitor
performance. Although nitrogen doping generally increases the electrical conductivity of carbon
because of a higher charge/electron carrier mobility [154-155], too much N can increase the
interfacial resistance too [156]. Moreover, the pseudocapacitive process contributed by the N
presence can blocks the original double layer capacitance (because the electrode surface does not
have a uniform charge distribution for the formation of the classic Helmholtz layer), resulting in a
lesser overall specific capacitance. A comparative study showed that the optimum amount of N
doping for an OMC ultracapacitor is about 6% [156].
In any case, N-doping can significantly improve the specific capacitance of OMC-based
ultracapacitors [154,157-163]. The surface of mesoporous silica template plays a substantial role in
the chemical structure of OMC, as can results in the formation N-rich surface having significant
redox system. This significantly improves the electrochemical performance [157]. The presence of
N adatoms and surface groups paves the path for new faradaic reactions, which can contribute to the
pseudocapacitive performance, e.g., by facilitating H insertion [164]. The specific capacitance of an
OMC-based ultracapacitor can be directly increased by increasing the presence of nitrogen while
the presence of oxygen functional groups has a slight influence [165].
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Although the role of N dopant is to cause chemical inhomogeneity, its influence depends on the
OMC architecture too. This effect is extremely higher for a 3D architecture of OMC (e.g., FDU-16),
as the specific capacitance is increased 7 times by N-doping [166]. While the original FDU-16
OMC is not considered as a promising material for ultracapacitors, N-doped FDU-16 OMC is
among the best candidates. The cyclability is impressive, as the specific capacitance is actually
increasing during the first 10,000 cycles due to the structural rearrangement opening new channels
for diffusion [166].
Another common dopant of carbon is boron [167]. Doping of OMC with boron also increases the
specific capacitance [168]. When substituting carbon, boron atoms are natively bonded with oxygen
atoms. The change in charge distribution across the carbon network and the oxygen functional
groups directly bonded with the OMC lattice causes a significant contribution of pseudocapacitance
in addition to the original double layer charging [169]. Nevertheless, this chemical reactivity results
in poor cyclability due to structural changes in the course of faradaic reactions [169].
While neighbor elements (B and N) just alter the uniformity of charge distribution across the carbon
network, doping with larger elements such as P can alter the morphology too resulting in substantial
changes in surface area and pore volume [170].
While hydrophilicity can improve the electrode wettability in electrochemical systems,
hydrophobicity can reduce corrosion. Doping of OMC with P increases the hydrophobicity, and
thus, protection against corrosion [171]. Sulfur functional groups can also contribute to the
pseudocapacitive behavior of OMC [172]. This also emphasizes that the influence of doping is not
only due to the presence of doping element in the carbon network (changing the charge distribution)
but also the functional groups formed on the dopant.
In fact, while the uniform architecture of OMC is beneficial for electrochemical performance,
chemical uniformity is not desirable, because chemical inhomogeneities of atoms at the
electrolyte/electrode interface facilitate charge transfer and electrochemical reaction. While gaining
the ordered structure of OMC, doping can create chemical inhomogeneity. Increasing this
inhomogeneity by multi dopants can significantly increase the specific capacitance; e.g., N/P
[170,173-174], B/P [175], N/S [176-179].
Although large surface area provides a significant double layer capacitance, the faradaic
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pseudocapacitance (or more precisely pseudocapacitive mechanism) of N-doped OMC is becoming
dominant at high dopant concentration [180]. Therefore, impedance spectroscopic spectra of N-
doped OMC represent the characteristics of faradaic systems with charge transfer semi-circle
followed by Warburg impedance.
An important issue, which is usually neglected, is the electrolyte solution. It is evident that
capacitive behavior is affected by the electroactive species due to their charge, but the influence of
size is of critical importance for OMC, as the sizes of hydrated/solvated ions are comparable with
that of mesopores. This means that some ions are larger or smaller than OMC mesopores, leading to
different capacitive behaviors [181-182].
It is worth to emphasize that nitrogen-doped nano-tubular ordered mesoporous few-layer carbon
(OMFLC) structure [80] has a large surface area (1580 m2/g), a large total pore volume (2.20 cm3
g–1), and an average pore width 2.25 nm. After composition optimization, a specific capacitance as
high as 855 F g–1 at a current density of 1 A g–1 was obtained in an aqueous solution of H2SO4
(Figure 9a,b). Ragone plot of energy vs. power densities of symmetric cells based on this material
in two different electrolytes (H2SO4 and Li2SO4) shows extraordinary performance when
comparing to other conventional batteries and supercapacitors (Figure 9c,d).
Figure 9. a) Cyclic voltammetry test and galvanostatic test of the cells using different components.
Ragone plot of specific energy vs. specific power in c) and energy density vs. power density in d) of
the cell performance, in comparision to other conventional batteries and supercapacitors. Reproduced
with permission from Ref.[80]. Copyright 2015, American Association for the Advancement of
Science.
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4.2. OMC for Pseudocapacitors
In pseudocapacitors, the so-called pseudocapacitance is the result of facile faradaic redox reactions
at the surface or sub-surface of the electroactive material. Better rate capability and
pseudocapacitive behavior are obtained when the ratio of surface reaction is significant in
comparison with the solid-state reaction. This dominance can be formed by increasing the specific
surface area; thus, a significant fraction of faradaic reaction is occurring at the surface with no need
for slow solid-state diffusion to reach the reactive redox sites, with the latter being characteristics of
charge storage in a battery.
Transition metal oxides are the common candidates for pseudocapacitors. Due to their electronic
insulating nature, carbon nanostructures are commonly used as a conductive framework for these
electroactive oxides. Increasing the specific surface area is indeed a common strategy in developing
electroactive materials for supercapacitors. High surface area nanocomposites with carbon is an
appropriate design, as nanostructured carbon can assist in distributing the electroactive material
while contributing to the electrical conductivity. In addition to common advantages of
carbonaceous nanomaterials, OMC can serve as an ideal template for the formation of
nanostructured electroactive material. Because of inter-connections of OMC pores, the electroactive
material is widely exposed to the electrolyte to shorten the diffusion paths by minimizing solid-state
diffusion [183].
OMC can chemically interact with the precursors for in situ synthesis of the electroactive
nanocomposites [184]. This is obviously accompanied by higher mechanical stability and
electrically conductivity. Owing to the mechanical stability of electroactive materials within the
OMC architecture, supercapacitors based on OMC nanocomposites shows practical cyclability over
thousands of cycles [185].
Conductive polymers are good candidates for supercapacitors, as their redox systems are normally
spread over wide ranges of potentials delivering pseudocapacitive behavior. Although diffusion
through polymer matrix is not very slow, it is still necessary to reduce the solid-state diffusion.
Interestingly, monomers can be injected within the OMC mesopores to initiate the polymerization
from within the pores [186]. Electrochemical polymerization of aniline has also been conducted
within the graphite interlayers [139]. The specific capacitance of OMC/polyaniline can be over 900
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F g-1 with an excellent cyclability over thousands of cycles in a 1 M H2SO4 electrolyte [186].
OMC/polyaniline show a good mechanical stability because of molecular interactions within the
nanocomposite matrix [187]. It has been shown that the rate capability of an OMC/polypyrrole
supercapacitor is about 50% better than pure polypyrrole [188]. OMC/PEDOT supercapacitor
showed only 14% capacity loss after 10,000 charge/discharge cycles [189].
The conductive polymer formed within the 3D meso-architecture of OMC can be the matrix for
additional electroactive materials too. The interesting feature is that all the reactants can chemically
interact for designing an in situ synthesis. For instance, polyaniline and manganese oxide directly
synthesized within OMC showed a good supercapacitor performance [190-192]. An extremely high
specific capacitance of 1668 F g–1 has been reported for ruthenium oxide/iron oxide embedded
within OMC in a 0.5 M H2SO4 electrolyte [193]. In general metal oxides embedded in OMC
display high specific capacitance [194].
It should be taken into account that the size of mesopores is somewhat comparable to the lattice size
of the electroactive material. Thus, the presence of an appropriate amount of reactants within the
mesopores is highly effective. For the case of metal oxide, the size, shape, and charge of the
reactant anion plays a substantial role in the structure and pseudocapacitive behavior of the metal
oxide formed within the OMC [118].
Comparison of 1D, 2D, and 3D OMCs made from different templates revealed that the ion mobility
significantly depends on the diffusion direction in an OMC/Fe2O3 nanocomposite. 1D architecture
showed the best rate capability in electrochemical performance, probably because of fewer
interactions between the diffusing species [195].
The presence of nitrogen heteroatoms in the structure of OMC can significantly improve the
interaction with electroactive materials resulting in enhanced specific capacitance [196].
4.3. OMC for Lithium Ion Batteries
The important roles of carbonaceous materials whether as active materials or conductive agents in
both anodes and cathodes of lithium ion batteries are evident. On the other hand, knowing the fact
that the main challenge of lithium batteries has always been related to the slow solid-state diffusion,
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the ordered interconnected channels of OMC can provide a new opportunity.
Most of the electrode materials of lithium ion batteries are poorly conductive. Carbon is a good
conductive agent, but it also blocks the Li diffusion. For instance, LiFePO4 is a promising cathode
material, but its needs a conductive agent to reach an acceptable conductivity for charge transfer
from the redox sites to the current collector. LiFePO4/OMC has been synthesized by a one-pot route
[197]. In this direction, OMC paves the path to employ novel candidates, which are not practical
standalone [198]. The 3D structure of OMC is an excellent matrix for the inclusion of electrode
materials for battery performance [199].
Synthesizing hollow OMC does not result in a high specific surface area (usually in the order of
500 m2 g–1), but as the outer structure has a better electrochemical accessibility, the material
displays a high rate capability for lithium ion batteries by reducing the struggles of Li cation in
solid-state diffusion [200-201].
The OMC scaffold provides an excellent matrix for the preparation of electroactive nanocomposites
as both anode [202-206] or cathode [197-198] materials. The majority of these nanocomposites are
prepared by in situ pore-filling approaches. In this case, the material density and mechanical
stability are high enough for practical applications.
In this direction, the OMC architecture is of key importance, as the diffusion of Li-ion is the rate-
determining step. Lithium battery performance of Sn nanoparticles embedded within an OMC with
larger pores and thinner pore walls has been reported to be better [159].
Most of OMCs are prepared based on silica templates, and the template removal can be a harmful
process. Quite interestingly, silica is a promising candidate as an anode material in lithium ion
batteries; and preparation of silica/carbon nanocomposites is an effective approach to overcome the
low electrical conductivity of silica. This suggests that the OMC and its template can be an active
anode material for lithium ion batteries [207]. In other words, this is indeed an in situ synthesis of a
highly ordered nanocomposite.
Pure OMC can be a candidate for anode material similar to other graphitic carbon nanomaterials.
However, the electrochemical performance is significantly poor in comparison with conventional
graphite in which Li can be intercalated [208]. In fact, although diffusion through mesopores is
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facilitated, intercalation within the carbon lattice is not favorable in the case of OMC.
In a similar fashion, OMC can be used as an electrode material for other metal ion batteries. For
instance, N-doped OMC has been utilized as an anode material in sodium ion battery [209].
4.4. OMC for Metal-Sulfur Batteries
Metal-sulfur batteries have recently attracted considerable attention due to their high specific
capacity resulting in an incredibly high energy density. The main challenge of this type of batteries
is the sulfur cathode. Since sulfur is non-conductive, cathode should be prepared by a conductive
agent. Like similar battery systems, carbon is the first choice as the conductive agent, and various
forms of carbon have been employed for the fabrication of Li-S cathodes [210-213]. Octasulfur
(cyclo-S8) is the common allotrope of sulfur, and its reduction into the final product of Li2S during
the discharge process is a stepwise process, producing Li2Sn (n = 4– 8) polysulfide intermediates
which are dissoluble in the electrolyte. The dissolved polysulfides shuttle between and react on the
sulfur cathode and lithium anode, resulting in a “chemical shortcut” inside the cell [214]. This
shuttle phenomenon causes irreversible loss of active materials, capacity fade, self-discharge, anode
etching, among many other detrimental effects. This is the most formidable challenges for the sulfur
cathode. Nazar and her coworkers prepared OMC/S as a promising cathode material for Li–S
batteries for the first time in 2009 [215]. The interesting feature of this idea is that sulfur can be
entrapped within the OMC structure if the pores are of the right size. This work started a new era in
developing Li-S batteries by physically trapping and chemically binding polysulfides in the cathode
matrix.
The point is that OMC provides a good permeability for the electroactive species; thus, sulfur can
be incorporated within the OMC structure [216-218]. This protects sulfur from dissolution while
electrochemically accessible. It is evident that the key challenge for improving the battery
performance of OMC/S cathodes is to control the morphology to increase the amount of sulfur
entrapment. In general, OMC particles of 200 – 500 nm with mesopores of 3 – 10 nm have shown
good battery performance with specific capacities over 1,000 mAh g–1.
The OMC scaffold can keep a high amount of sulfur, ca. over 50% therein [219]. Owing to the
mechanical stability of entanglement within the interconnected mesopores, the OMC cathode
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displays an excellent cyclability. Since sulfur is not a concrete electrode material with a rigid
structure like metal oxides, it is subject to severe dissolution. The size of OMC mesopores well fits
with the S8 structure formed therein, and thus, OMC/S cathode shows an excellent cyclability in
comparison with other carbonaceous materials [220]. However, the performance is not
straightforward in practice, as the irreversible inclusion of sulfur within microporosity of the
mesopores results in a severe capacity fading. As a matter of fact, OMC can be a good candidate as
an S electrode if its architecture is thoroughly designed.
In addition to physically entrapping of polysulfides to retard their diffusion out of the cathode, To
further protect the release of sulfur, binding these polar species chemically onto the carbon matrix is
another strategy. Since carbon itself is intrinsically non-polar with a less binding capability to the
polar polysulfides, surface functionalization of OMC, including heteroatom doping, conductive
polymer or transition metal oxides and sulfides decoration can dramatically enhance the binding
capability of OMC to polysulfides [221]. With a surface of S-embedded OMC covered by a
conductive polymer, a high specific capacity over 1,000 mAh g–1 is achieved with an acceptable
capacity retention for over 1000 cycles [222]. Using PEDOT decorated ordered mesoporous carbon
nanocube to load sulfur, Wang et al. [223] demonstrated a sulfur cathode with large capacity, long
cycling stability and high rate capability (Figure 10).
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Figure 10. (a) Schematic of PEDOT decorated mesoporous carbon nanocubes for sulfur cathode. b)
Cycling performance of at 0.5C and 5C and the corresponding Coulombic efficiencies. Reproduced
with permission from Ref.[222]. Copyright 2015, Elsevier.
4.5. OMC for Li-Air Batteries
In metal-air batteries, such as Li–O2, the key challenge is the porous catalytic cathode material in
which Li2O2 is formed and decomposed. It forms the bottleneck since the sluggish ORR/OER
kinetics increase the overpotential and limit the recharge capacity and rate performance. The
insoluble discharge product (Li2O2) will gradually block the flow of electrolyte and O2. It has been
demonstrated that the OMC skeleton is suitable for the formation of Li2O2 [224]. The ordered
matrix of OMC provides an opportunity for uniform distribution of catalyst nanoparticles. This is of
particular importance, as metallic nanoparticles should not block the Li diffusion, which is the main
charge carrier. Using an ordered hierarchical mesoporous/macroporous carbon, a high-performance
cathode was demonstrated [112].
The cathode of metal-air batteries resembles fuel cells and needs ideal electrocatalysts for both
oxygen evolution reaction (OER) and oxygen reduction reaction (ORR) during the charge and
discharge processes, respectively. Whether employing the classical Pt catalyst or a new alternative
such as metal oxides [225], a key requirement is a uniform distribution of the catalyst over the
catalyst support to make the catalyst more accessible electrochemically. Using OMC as
electrocatalyst will be summarized in section 4.6. Wang et al. fabricated a three-dimensional
ordered mesoporous carbon by growing a thin layer of FeOx using atomic layer deposition; when
decorated with Pd nanoparticle catalysts, the new cathode exhibits a capacity greater than 6000
mAh/g and cyclability of more than 68 cycles [224]. Figure 11 shows the morphological structure
and the performance of OMC/FeOx/Pt electrode.
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Figure 11. a) Schematic of the catalyst loaded OMC structure. b) Pore size distribution change after
FeOx coating. c) TEM images of pristine OMC, after FeOx coating, and after Pd NP decoration. d)
Schematic illustrating the influence of Li2O2 deposition on the ORR activity of carbon and the
subsequent effects of the FeOx coating and Pd NP decoration. e) Cycling curves for the bare, FeOx
coated, and Pd decorated OMC electrodes. Reproduced with permission from Ref.[224]. Copyright
2015, Wiley-VCH.
Although the current focus is on Li–O2 battery among metal-air batteries, the possibility of
employing OMC is not limited to Li–O2 only. For instance, OMC has been successfully employed
for other metal-air cells such as Zn-air cells [226].
4.6. OMC as Electrocatalyst Support
Electrocatalysts participate in electrochemical reactions by lowering the reaction activation energy
and by lowering the excess energy consumed by the activation barrier. They playing critical roles in
the electrochemical fuel (H2, CO, CH4, etc.) production and energy generation (e.g., in fuel cells).
A wide range of electrochemical systems utilizing Pt or similar precious metals or transition metal
oxides as an electrocatalyst. The role of catalyst support is critically important in these systems to
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fairly disperse the catalysts to improve the system efficiency and reduce the amount of expensive
catalyst required. Carbon is an ideal catalyst support because of its electrical conductivity and high
specific surface area, and mesoporous structure is the best choice for two reasons: simultaneous
synthesis of the catalyst can result in the formation of uniform nanoparticles over the mesopores as
a template, and catalyst nanoparticles can be uniformly distributed over the mesoporous structure.
However, preparation of carbon/catalyst nanocomposites is not as easy as it seems; a significant
part of the catalyst is actually covered by carbon and becomes electrochemically inaccessible [227-
228].
A preliminary study showed that OMC capability for dispersing Pt nanoparticles is higher than
those of similar carbon nanomaterials [229]. This named OMC as a promising catalyst support for
various applications, particularly fuel cells. The morphology of micropores is basically responsible
for the desirable arrangement of metallic catalysts to be well dispersed while electrochemically
accessible [230]. In addition to the physical entrapment of metallic nanoparticles within the OMC
scaffold, chemical interactions can also improve the catalytic activity of OMC supported Pt [231].
Functionalizing OMC with oxygen groups can assist in anchoring Pt catalyst while preserving the
originally ordered structure [232]. For the electrochemical oxidation of CO, this reduces the
overpotential about 100-150 mV. Although the fundamental mechanism for this improvement has
not been elaborated yet, similar values for various OMCs have been reported by different authors
[232-233].
Quite interestingly, the catalytic activity of OMC-supported Pt depends on the OMC architecture
rather than mesopore size [234]. Figure 12 compares the structure and electrocatalytic activities of
two OMCs having inverse structure; while one is an excellent catalyst support, the other is quite
poor.
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Figure 12. (a) Schematic model, (b) TEM images and (c) electrocatalytic activities of two OMC
samples synthesized using CMK-3 and FDU-15 templates. Reproduced with permission from
Ref.[234]. Copyright 2011, Royal Society of Chemistry.
Pt/OMC nanocomposites show excellent electrocatalytic behavior, e.g., for fuel cells [235-237].
The electrocatalytic activity of Pt catalyst supported by OMC for oxygen reduction is two times
higher than that supported by commercial conductive carbon [238]. Similar behavior has been
reported for the electrocatalytic activity of Pd in alkaline fuel cells[239].
It has been reported that in the preparation of OMC-supported Pt/Ni bimetallic catalyst, the amount
of Ni controls the surface hydroxyl groups, which cause hydrophilicity of the OMC catalyst support
[240]. This significantly enhances the electrocatalytic activity for the oxidation of methanol by
facilitating the formation of Pt-OH. Another important phenomenon is that increasing the Ni
content reduces the size of bimetallic nanoparticles, which can become smaller than the size of
mesopores. This is accompanied by a better distribution of Pt and higher accessibility. This
enhanced electrocatalytic activity of the bimetallic catalyst is not limited to Ni. PtFex, for example,
displays exactly similar behavior [241]. A vital necessity for optimum electrocatalytic activity is the
integrity of bimetallic nanoparticles over the OMC matrix. The shape and size of nanoparticles
should match those of mesopores.
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OMC is a good compositing agent for metal oxides, which are promising candidates for ORR
electrocatalysis, due to the interaction of oxygen groups [242-243].
Nitrogen doping improves the properties of OMC as a catalyst support due to the presence of
nitrogen coordinated metal centers [140]. This can facilitate platinum-free electrocatalyst [244]. As
explained for the case of supercapacitors, bi-dopants can further contribute to the chemical
inhomogeneity of OMC resulting in better charge transfer in electrocatalytic reactions [245]. The
electrocatalytic activity of nitrogen and sulfur co-doped OMC is comparable with that of Pt/C for
ORR [246]. Doping of OMC with N and a metal can lead to superior electrocatalysts. N and Fe co-
doped OMC shows a superior electrocatalytic activity for ORR, even stronger than that of Pt [247].
However, the influence of doping is not straightforward as several factors are changed
simultaneously. Figure 13 shows the effect of N-doping on Pt/OMC and Pt-Co/OMC
electrocatalysts. Contrary to the enhanced capacitive behavior of N-doped OMC described before,
N doping of Pt/OMC reduces both capacitance and electrocatalytic activity. However, N-doping
strongly improves both capacitive and electrocatalytic activity of Pt-Co/OMC. This can be ascribed
to several factors. The presence of Co can enhance the graphitization of OMC. As discussed for the
bimetallic catalysts before, the presence of Co results in smaller nanoparticles, which are
comparable with the mesopore sizes [68]. Therefore, the systems are significantly different. This
difference is more visible for direct electrochemical oxidation at the electrocatalysts (Figure 13b). N
doping strongly improves the electrocatalytic activity of Pt-Co/OMC but at the price of higher
overpotentials, due to the electrochemical redox systems of N-rich functional groups.
Figure 13. CV curves of Pt/OMC, Pt/N-OMC, Pt/Co-OMC, and Pt/Co-N-OMC samples in 0.5 M
H2SO4 (a) and 2.0 M CH3OH 1.0 M H2SO4 (b) with a scan rate of 20 mV s-1. Reproduced with
permission from Ref.[68]. Copyright 2013, American Chemical Society.
The electrocatalytic capability of OMC is not limited to catalyst support, as it can be directly used
as a metal-free catalyst [248]. For this purpose, it is necessary to alter the lattice and surface
structure of OMC by doping and surface functionalization. Doping of OMC with various elements
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such as boron [249], sulfur [250], etc. showed an acceptable electrocatalytic activity for ORR.
Similar to the case of supercapacitors, co-doping can further improve the electrocatalytic activity of
OMC [251].
Although OMC is chemically stable in various media including the alkaline electrolyte, there is a
gradual decrease in catalytic activity. In the case of pure OMC, the capacitive behavior is weakened
while pseudocapacitive behavior is strengthened, because of the formation of reactive defects and
functional groups. For doped OMCs in which there are active redox sites, aging cause a decrease in
chemical reactivity [252].
The ordered mesoporous structure of OMC provides an excellent opportunity for the formation of
1D catalysts within the OMC structure. This feature has been utilized for in situ synthesis of various
catalysts supported on OMC[253-254].
Since the pores are usually long along the OMC structure, diffusion of electroactive species is
normally unidirectional. Modifying OMC by carbon nanotubes can create shortcuts for charge
transfer perpendicular to the pores, and thus, significantly improve the electrocatalytic activity
[119,181]. Since the electrocatalytic activity is not controlled by the amount carbon nanotubes,
carbon nanotubes are not real channels for diffusion, but shortcuts opening gates in other directions
(for charge transfer rather than ion diffusion) [255]. The same behavior has been reported for
OMC/CNT architecture as an ultracapacitor [256]. This is similar to the phenomenon reported for
electrodeposition in the presence of carbon nanotubes in which the presence of carbon nanotubes
within the diffusion layer just changes the electrodeposition pathway without physical entrapment
in the depositing film [257-258]. Although the silica/carbon nanocomposite was originally an
intermediary template, it can be prepared as a free-standing film with excellent casting capability
for practical applications [259].
4.7. Electrochemical Hydrogen Storage
Hydrogen is ideally the greenest fuel, but its applications have been limited by difficulties in
storage. In the past two decades, carbon was a promising candidate to store hydrogen in lieu of
metal hydrides storing hydrogen in bulk. Thus, the surface structure of carbon is of particular
importance to achieving an acceptable hydrogen storage capacity. A key problem in hydrogen
Page 35 of 56
storage on carbon surface is that adsorbed H atoms can interact with each other to form H2 and
leave the material in gaseous form. OMC seems a promising candidate, as adsorbed atoms are
somehow entrapped within the mesopores. In addition to the morphological structure, chemical
functionality also plays a substantial role in the hydrogen storage capacity of OMC. It has been
reported that while oxidized nitrogen functional groups may prevent the adsorption of hydrogen, N-
doped OMC showed 1.5 times enhancement in electrochemical hydrogen storage [260-261].
While OMC stores hydrogen by surface interaction, metals can store hydrogen in the form of metal
hydride. Mixing metal nanoparticles with OMC can assist catalytic hydrogen to dissociate for
absorption on the carbon surface while contributing to the hydrogen storage in the form of metal
hydride. Ni/OMC nanocomposite showed a good capacity for electrochemical hydrogen storage
[262]. As mentioned above, Ni can improve the hydrophilicity nature of OMC due to the hydrogen
functional groups. The capability of an OMC-supported Pt/Ni for electrochemical hydrogen storage
is increased three times when the Ni content is increased from 2 to 15% [240]. Similar behavior has
also been observed for OMC-supported NiFe too [263].
There is a great flexibility for doping of OMC targeting electrochemical applications. Cu and N
were utilized as dopants to improve the capacity of OMC for electrochemical hydrogen storage
[264].
5. Summary and Outlook
OMC has attracted considerable attention during the past years for potential applications in
various electrochemical energy storage and conversion systems. However, a possible misleading is
that OMC is somewhat considered as a standard material with well-defined architecture. In practice,
at least in electrochemical systems, OMCs are very complicated materials which represent some
kind of order at a mesoscale. Both the chemical structure of the pore walls and edges are critically
important in electrochemical systems, but less attention is usually paid to compare similar OMCs in
a specific application. On the other hand, not only the interconnection of the mesopores is of
essential importance, the packing of the material particles can define the overall accessibility of the
mesopores. In other words, in a compact electrode, the OMC architecture is not as ordered as seen
in the TEM images.
Page 36 of 56
Along with the growing interest in OMC, there have appeared reports in the literature claiming the
unsuitability of OMC for many electrochemical systems. Here, we attempted to highlight two
aspects of this potential material: (i) it is a fact that OMC is not as charming and ideal as it is seen
in TEM images, and (ii) possible weak performance in electrochemical systems is not necessarily
incapability of OMC for conducting the electrochemical reaction within its ordered architecture. In
general, OMC should be specifically tuned for various applications including those of
electrochemical energy storage and conversation. Some of the reports available in the literature
clearly show the potentials of OMC for various electrochemical systems, but the "one size fits all"
strategy does not work here.
The main obstacle for the practical application of OMC in electrochemical energy systems is the
lack of an appropriate synthesis route for mass production of OMC while designing its architecture
for the electrochemical cell. While the conventional silica template method is ideal for the
preparation of highly ordered mesopores at a lab scale, there is still no practical approach for
scaling up this synthesis route. On the other hand, soft-templates methods or other hard templates
are more practical for the mass production, but at the cost of losing the highly ordered architecture
of OMC to some extent. Combining these methods might be the subtle approach for the practical
production of OMC. Owing to the essential importance of the pore directions in the OMC
architecture, not only the synthesis but also the arrangement of the OMC particles in the electrode
composite is of practical importance. Therefore, the OMC should be prepared as a film or directly
grown on the current collector to guarantee the original electrochemical properties. In conclusion,
we need more fundamental studies to understand how the OMC atomic structure is controlling the
electrochemical processes, instead of typical examinations of OMCs in different systems.
Acknowledgements
Z.F. acknowledges the support from the National Science Foundation (1611060).
Page 37 of 56
Figure Captions
Figure 1. Schematic comparing a) hard-template based and b) soft-template based synthesis
strategies. Reproduced with permission from Ref.[19]. Copyright 2006, Wiley-VCH.
Figure 2. a) Schematic of MGB synthesis from drop-casting functionalized beads/FeCl3 solution, to
thermal annealing for graphene growth, and etching away Fe domain to obtain MGB. b,c) TEM
images of MGB. Reproduced with permission from Ref.[78]. Copyright 2013, American Chemical
Society.
Figure 3. a) Schematic of the OMG synthesis from colloidal Fe3O4 NPs. b,c) TEM images of the
as-synthesized OMC superlattice after catalytic carbonization at 500 oC with fcc symmetry. d,e)
TEM images of OMG after further graphitized at 1000 oC, imaged for (111) plane. Reproduced
with permission from Ref.[22]. Copyright 2015, Wiley-VCH.
Figure 4. a) Schematic to synthesize nitrogen doped OMG. b) Low-angle x-ray diffraction patterns
of the synthesized sample with or without N-doping, showing the characteristic peaks of hexagonal
packing. Reproduced with permission from Ref.[80]. Copyright 2015, American Association for the
Advancement of Science.
Figure 5. a) Schematic of CMK-3G OMG consisting of hexagonal arrays of carbon nanorods,
while the nanorods is formed by a stacking of the discoid graphene sheets oriented perpendicular to
the rod orientation. b) TEM images of CMK-3G showing the rod array. c) TEM images showing
the stacked discoid graphene sheets. The inset is the corresponding electron diffraction pattern.
Reproduced with permission from Ref.[83]. Copyright 1971, The Electrochemical Society.
Figure 6. SEM and TEM images of the ordered hierarchical mesoporous/macroporous carbon at
different scales. Reproduced with permission from Ref.[112]. Copyright 2013, Wiley-VCH.
Figure 7. An illustration for designing carbon-supported Pt electrocatalyst with
macroporous/mesoporous architecture. Reproduced with permission from Ref.[113]. Copyright
2015, Wiley-VCH.
Figure 8. (a-h) SEM and TEM images of an N-doped OMC with Im3m symmetry and rhombic
Page 38 of 56
dodecahedral single crystal morphology. (i) Cyclic voltammograms and (j) charge/discharge
profiles of the N-doped OMC as an ultracapacitor. Reproduced with permission from Ref.[125].
Copyright 2015, Royal Society of Chemistry.
Figure 9. a) Cyclic voltammetry test and galvanostatic test of the cells using different components.
Ragone plot of specific energy vs. specific power in c) and energy density vs. power density in d) of
the cell performance, in comparision to other conventional batteries and supercapacitors.
Reproduced with permission from Ref.[80]. Copyright 2015, American Association for the
Advancement of Science.
Figure 10. (a) Schematic of PEDOT decorated mesoporous carbon nanocubes for sulfur cathode. b)
Cycling performance of at 0.5C and 5C and the corresponding Coulombic efficiencies. Reproduced
with permission from Ref.[222]. Copyright 2015, Elsevier.
Figure 11. a) Schematic of the catalyst loaded OMC structure. b) Pore size distribution change after
FeOx coating. c) TEM images of pristine OMC, after FeOx coating, and after Pd NP decoration. d)
Schematic illustrating the influence of Li2O2 deposition on the ORR activity of carbon and the
subsequent effects of the FeOx coating and Pd NP decoration. e) Cycling curves for the bare, FeOx
coated, and Pd decorated OMC electrodes. Reproduced with permission from Ref.[224]. Copyright
2015, Wiley-VCH.
Figure 12. (a) Schematic model, (b) TEM images and (c) electrocatalytic activities of two OMC
samples synthesized using CMK-3 and FDU-15 templates. Reproduced with permission from
Ref.[234]. Copyright 2011, Royal Society of Chemistry.
Figure 13. CV curves of Pt/OMC, Pt/N-OMC, Pt/Co-OMC, and Pt/Co-N-OMC samples in 0.5 M
H2SO4 (a) and 2.0 M CH3OH 1.0 M H2SO4 (b) with a scan rate of 20 mV s-1. Reproduced with
permission from Ref.[68]. Copyright 2013, American Chemical Society.
Page 39 of 56
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