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DOI: 10.1002/cssc.201200990
Porous Graphitic Carbon Nanosheets Derived from
Cornstalk Biomass for Advanced Supercapacitors
Lei Wang,[a, b] Guang Mu,[a] Chungui Tian,[a] Li Sun,[a] Wei Zhou,[a] Peng Yu,[a] Jie Yin,[a] and
Honggang Fu*[a, b]
Porous graphitic carbon nanosheets (PGCS) are synthesized by
an in situ self-generating template strategy based on the car-
burized effect of iron with cornstalks. Cornstalks firstly coordi-
nate with [Fe(CN)6]4 ions to form the cornstalk–[Fe(CN)6]4
precursor. After carbonization and removal of the catalyst,
PGCS are obtained. Series experiments indicate that PGCS can
only be formed when using an iron-based catalyst that can
generate a carburized phase during the pyrolytic process. The
unique structures of PGCS exhibit excellent capacitive perfor-
mance. The PGCS-1-1100 sample (synthesized from 0.1 m
[Fe(CN)6]4 with a carbonization temperature of 1100 8C), which
Introduction
Crop stalks are a type of natural cellulosic biomass, which
could be considered as the most valuable and abundant
renewable resource on earth.[1, 2] In China, the annual yield of
natural cellulosic biomass exceeds 700 million tons, of which
cornstalks account for over 30 %.[3] As a natural resource, corn-
stalks contain a rich nutritional and chemical composition,
which has attracted special attention to cornstalks in industry,
agriculture, and animal husbandry. Accordingly, about 50 % of
cornstalks have been used to produce feeds and fertilizers, and
approximately 30 % of cornstalks are used as the fuel and the
industrial feedstock for the production of alcohol, hydrogen,
and methane.[4–7] However, huge amounts of cornstalks are still
left in harvested fields without further utilization, which leads
to various environmental problems, and more importantly, re-
sults in the waste of renewable resources. Because of the strat-
egy of sustainable development, combined with the original
concept of “waste-to-wealth”, the potential application of corn-
stalks in materials science is attracting a large amount of atten-
tion.[8, 9] Therefore, it is very important to convert cornstalks
into carbon materials with specific structures because of the
[a] Dr. L. Wang, Dr. G. Mu, Dr. C. Tian, Dr. L. Sun, Dr. W. Zhou, P. Yu, J. Yin,
Prof. H. Fu
Key Laboratory of Functional Inorganic Material Chemistry
Ministry of Education of the People’s Republic of China
Heilongjiang University, Harbin 150080 (PR China)
Fax: (+ 86) 451-8666-1259
E-mail: fuhg@vip.sina.com
[b] Dr. L. Wang, Prof. H. Fu
State Key Laboratory of Theoretical and Computation Chemistry
Jilin University, Changchun 130023 (PR China)
Supporting Information for this article is available on the WWW under
http://dx.doi.org/10.1002/cssc.201200990.
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shows excellent electrochemical capacitance (up to 213 F g1
at 1 A g1), cycling stability, and rate performance in 6 m KOH
electrolyte. In the two-electrode symmetric supercapacitors,
the maximum energy densities that can be achieved are as
high as 9.4 and 61.3 Wh kg1 in aqueous and organic electro-
lytes, respectively. Moreover, high energy densities of 8.3 and
40.6 Wh kg1 are achieved at the high power density of
10.5 kW kg1 in aqueous and organic electrolytes, respectively.
This strategy holds great promise for preparing PGCS from nat-
ural resources, including cornstalks, as advanced electrodes in
supercapacitors.
rich carbonaceous species that are contained within them.
Unfortunately, cornstalks have only been utilized as the feed-
stock to synthesize activated carbon materials that only have
one application, that is, as gas adsorbents.[10] Cornstalks are
composed of three main fractions, namely, cellulose, hemicellu-
lose, and lignin, which contain abundant polar hydroxyl and
carbonyl groups (see Figure S1).[2] Such characteristic features
enable cornstalks to coordinate with various metal ions, which
can be used for the synthesis of carbon materials.[11–13] These
properties enable cornstalks to be an effective feedstock for
carbon materials with specific structures for certain fields.
Electrochemical double layer capacitors (EDLCs, also called
supercapacitors) that use carbon as the active material, are
a class of device for electrical energy storage with high power
densities, long lifespans, as well as rapid capture and storage
of energy.[14–18] The energy is stored at the electrolyte/carbon
interface by charging of the double-layer capacitance through
the reversible ion adsorption on the carbon surface.[19–21] Thus,
carbon materials with large Brunauer–Emmett–Teller (BET) spe-
cific surface areas (SBET) are very important for high-perfor-
mance EDLCs. However, activated carbon materials with a very
high SBET (above 2000 m2 g1) only exhibit a limited improve-
ment in capacitance because ion and electron transport are
confined by the low mesoporosity and poor electronic conduc-
tivity of the material.[22] Many efforts have recently been fo-
cused on preparing improved electrode materials with porous
structures and good electronic conductivity; porous electrode
structures can increase the number of interactions between
the electrolyte ions and the electrode by decreasing the ion-
transport resistance and diffusion distance, whereas good elec-
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tronic conductivity of electrode can increase electron transport

at the electrode.[23–27]
Recently, 2D carbon nanomaterials with porous structures
have attracted tremendous attention in the area of EDLCs
owing to them possessing excellent electronic transportation
properties, such as that of graphene.[28, 29] Additionally, we re-
cently discovered that the mesoporous carbon coating on gra-
phene and graphite nanosheets with high SBET and suitable Scheme 1. Image of the PGCS, indicating that the porous structures could
pore sizes show excellent electrochemical capacitance and cy- allow free ion insertion/extraction and that the graphitic carbon nanosheets
[30, 31] could supply a direct path for electrons transport.
cling stability. The successes have inspired us to synthesize
porous graphitic carbon nanosheets (PGCS) as electrodes for
EDLCs. To limit environmental pollution and resource scarcity, for applications in materials science, which does not compete
it is important to develop an economic method for preparing with food sources and is widely available as a low-cost feed-
PGCS for EDLCs that are derived from biomass such as corn- stock.
stalks.
The polar groups (i.e., carboxyl and hydroxyl) in the cellu-
lose, hemicellulose, and lignin from cornstalks have previously Results and Discussion
been shown to coordinate with various metal ions.[11–13] Our
The structures of PGCS
previous study demonstrated that the generation of planar ce-
mentite could be beneficial for the formation of 2D-layered To synthesize PGCS, cornstalks were firstly immersed into
carbon nanostructures.[12] Herein, we present a template-free K4[Fe(CN)6] aqueous solutions for 4 h. The cornstalk-[Fe(CN)6]4
route to synthesize PGCS derived from cornstalks based on the composite was then obtained through a coordination effect
carburized effect of iron. The template-free route means that between the cornstalks and [Fe(CN)6]4 ions. After carboniza-
the catalyst itself acts as the template; this is also referred to tion had occurred under argon and the catalyst was removed
as an in situ self-generating template. In the synthesis, the by using hydrochloric acid, the PGCS were prepared. The
cornstalks are firstly coordinated with [Fe(CN)6]4 to form sample notation and synthesis conditions are displayed in
a cornstalk–[Fe(CN)6]4 composite. After carbonization and re- Table S1. Further insight into the detailed microstructure of the
moval of the catalyst, PGCS are obtained. To the best of our sample was elucidated by using TEM. Figure 1 displays TEM
knowledge, we demonstrate the synthesis of PGCS from natu- images of PGCS-1-1100, which was synthesized from
ral sources for the first time. Series experiments demonstrate 0.1 m K4[Fe(CN)6] and carbonized at 1100 8C. It was observed
that the selection of a suitable catalyst plays a key role in the that the sample was composed of nanosheets with a mesopore
formation of PGCS. The unique structure of the resultant PGCS size between 2 and 9 nm, which is a favorable size for applica-
allows for good performance in EDLCs, as illustrated in tions in the field of supercapacitors. Moreover, the high resolu-
Scheme 1. Firstly, the highly
porous structure is beneficial for
electrolyte accessibility and rapid
ion diffusion/transport by pro-
viding a short ion-diffusion dis-
tance. Secondly, the excellent
conductivity of the 2D planar
nanosheets with graphitic nano-
structures are shown to facilitate
fast electron transport during
electrochemical processes. Final-
ly, independent of the way in
which the PCGS are connected,
that is, in parallel or in series, the
PGCS, which act as mini current
collectors, can form an overall
conductive network in the elec-
trode. The synthesized PGCS can
be used as electrodes for ad-
vanced supercapacitors with ex-
cellent capacitive performances.
Figure 1. TEM images of the as-synthesized PGCS-1-1100 sample: (a) the overall structure of the sample, (b, c) the
Our work demonstrates that
enlarged structures of the selected area in (a), (d) the enlarged structure of the selected area in (c), (e) the en-
cornstalks can be widely utilized larged structure of the selected area in (d); pores with a PSD of about of 2 and 9 nm can be observed clearly
as a natural renewable material (signed by white circles), and (f) the HRTEM image of the selected area in (c).

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tion TEM (HRTEM) image shows the distinct lattice distance of
graphite (001), which implied the presence of well-graphitized
structures beneficial for electron transport. The above analyses
indicated that samples containing PGCS were successfully
synthesized.
The XRD pattern of PGCS-1-1100 exhibits the (002), (100)
and (004) graphite diffraction peaks, see Figure 2 a, which indi-
cated that the synthesized sample had good crystallinity; this
Figure 2. (a) XRD patterns and (b) Raman spectra for the PGCS samples syn-
thesized under various conditions. The produced carbon materials were
labeled according to the catalyst concentration and the carbonization tem-
perature, see the Experimental Section for details.
was consistent with the TEM results. Studies of samples de-
rived from different catalyst concentrations and different car-
bonization temperatures were also performed for comparison.
It was concluded that all samples synthesized by using this
strategy presented high crystallinity from the strong character-
istic diffraction peaks of graphite. Furthermore, the d-spacing
(d002), lateral size (La), and stacking height (Lc) were also calcu-
lated (Table S2). When the catalyst concentration or the car-
bonization temperature was increased, the d002 values de-
creased, whereas the La and Lc values increased. Crystallite
sizes (La and Lc) increase with decreasing d002 because the crys-
tallinity of the samples increase.[32, 33] The decrease in d002 with
an increase in catalyst concentration and carbonization tem-
perature could be attributed to the development of stacking,
which produced a more graphitic structure.[34] It was observed
that PGCS-1-1100 had a more compact structure, similar to
that of a graphite layer (d002 for the graphitic structure was
0.335 nm).
To further evaluate the crystallinity of the carbon materials,
the samples were characterized by using Raman spectroscopy,
the results are shown in Figure 2 b. The PGCS-1-1100 sample
exhibited the three typical bands, that is, the G band
(1575 cm1), D band (1361 cm1), and 2D band (2725 cm1).
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The G band is characteristic of the vibration of sp2-bonded
carbon atoms in a 2D hexagonal lattice (E2g mode). The D
band is associated with the vibrations of carbon atoms with
dangling bonds for the in-plane terminations of disordered
graphite. The second-order 2D band is typical of graphitic
carbon.[35] The intensity ratio between the G and D bands
(IG/ID) is proportional to the graphitization degree of carbon
materials (Table S3). The PGCS-1-1100 sample demonstrated
a high IG/ID value of 1.6, suggesting high crystallinity consistent
with the TEM imaging. The high crystallinity could facilitate
electron transport during charging–discharging of supercapaci-
tors. Moreover, the samples derived from different catalyst con-
centrations and different carbonization temperatures were also
analyzed for comparison. All of the PGCS samples exhibited
narrow D and G bands, and intense 2D bands, symbolic of
graphitic carbon with high crystallinity. Additionally, the value
for the ratio of IG/ID increased with increasing catalyst concen-
tration and carbonization temperature, which implied that the
crystallinity of the resultant PGCS also increased.
The structure of the PGCS samples were further investigated
by conducting N2 sorption isothermal analysis; the results are
shown in Figure 3 and the corresponding adsorption parame-
Figure 3. (a) N2 adsorption–desorption isotherms at 196 8C and (b) the cor-
responding NLDFT PSD curves for the PGCS samples.
ters are displayed in Table 1. The typical type IV isotherms with
H3 hysteresis loops indicate the presence of slit-like pores,
which are the characteristic of platelet structures.[36] It was fur-
ther demonstrated that the PGCS samples exhibit the struc-
tures of planar nanosheets. Moreover, hysteresis loops at P/Po
values between 0.5 and 0.9 implied that mesopores existed
within the samples. These results were confirmed by calculat-
ing the pore size distribution (PSD) by using the nonlocal den-
sity functional theory (NLDFT) method (inset in Figure 3 b),
which demonstrated bimodal mesopore sizes of 2.3 and
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Table 1. Adsorption parameters calculated from N2 adsorption isotherms
at 196 8C.
Samples SBET [m2 g1][a] Vt [cm3 g1][b] w [nm][c]
PGCS-05-1100 326 0.25 2.4,
PGCS-1-1000 788 0.63 2.4,
PGCS-1-1100 540 0.48 2.3,
PGCS-1-1200 474 0.41 2.3,
PGCS-3-1100 496 0.43 2.3,
AC-1100 0.6
[a] SBET calculated from the BET equation. [b] Vt is the single-point pore
volume from adsorption isotherms. [c] w is the mesopore diameter at the
maximum of the PSD curves, calculated according to the adsorption
branch of the isotherm by using the NLDFT method.
9.2 nm, consistent with the above TEM images. The
PGCS-1-1100 sample exhibited a SBET of 540 m2 g1. Moreover,
the lowest and highest SBET values were demonstrated in
PGCS-05-1100 and PGCS-1-1000, respectively, which were ap-
proximately 326 and 788 m2 g1. It could also be concluded
that the SBET value decreased consistently with increasing cata-
lyst concentration and carbonization temperature. Therefore,
the SBET values decreased with increasing crystallinity in the
PGCS samples. It was anticipated that PGCS-1-1100 would ex-
hibit excellent capacitive performance owing to its moderate
crystallinity, SBET value, and pore size. The presented synthetic
strategy demonstrated the following advantages: (i) PGCS
could be produced from the natural biomass of cornstalks,
(ii) PGCS could be synthesized without any additional porogen,
in the absence of a template, (iii) it was simple and cost-effec-
tive, and (iv) the synthesized PGCS materials exhibited bimodal
structures and high crystallinity. The above characteristics ena-
bled the PGCS to be considered for supercapacitor applica-
tions.
Formation mechanism
2D graphene-like structures are generally formed by using
a planar template. For example, the chemical vapor deposition
(CVD) method utilizes planar Ni and Cu substrates as templates
for the limited growth of graphene.[37, 38] In this study, the PGCS
were obtained by carbonizing the cornstalk-[Fe(CN)6]4 compo-
site and subsequently removing the catalyst. No substrate was
adopted during the synthesis. Understanding the formation
process of PGCS enables the controllable synthesis of carbon
nanostructures that could be tailored for use in different fields.
The type of catalyst used could affect the structure of the re-
sultant carbon materials. To study this effect, FeCl2 solution
was used as the catalyst instead of K4[Fe(CN)6] solution (the
composite of cornstalk-Fe2 + was formed after coordination),
followed by carbonization and subsequent hydrochloric acid
treatment. Figure S2 displays the TEM images of the as-synthe-
sized GC-FeCl2-1100 sample. It was observed that graphitic
carbon nanocapsules could be obtained, but not PGCS.
According to previous reports, Fe-, Co-, and Ni-based compo-
nents could be used as the catalysts for the synthesis of graph-
itic carbon. To study the effect of the catalyst on the morphol-
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ogy of the carbon nanostructures, CoCl2 and NiCl2 solutions
were used as the catalyst instead of K4[Fe(CN)6] solution. After
coordinating each catalyst with cornstalks, the cornstalk-Co2 +
and cornstalk-Ni2 + composites were formed, and subsequent
9.2 carbonization and hydrochloric acid treatment yielded the
9.1 GC-CoCl2-1100 and GC-NiCl2-1100 samples, respectively. Ac-
9.2
cording to the TEM images (Figure S2), graphitic carbon nano-
9.2
9.2 capsules were obtained. Notably, the SBET values for the carbon
nanocapsules prepared from different catalysts were in the
range of 34–184 m2 g1 (Figure S3), which were much lower
than that of the PGCS samples (326–788 m2 g1). The difference
was attributed to the different structure of these materials.
Moreover, the cementite phase (Fe3C) was generated during
the pyrolysis of cornstalk-[Fe(CN)6]4, as demonstrated by the
XRD results (Figure 4), which was not be detected by pyrolyz-
ing the cornstalk-Co2 + or cornstalk-Ni2 + composites (see Fig-
ure S4, in the Supporting Information, for detailed XRD analy-
sis). It was concluded that the generation of cementite (Fe3C)
and the following exuded process (i.e., to obtain Fe and C
from Fe3C) were significant for the formation of PGCS.
Figure 4. XRD patterns for samples derived from the cornstalk-[Fe(CN)6]4
composite, synthesized over a carbonization temperature range of 700–
1100 8C.
Based on the above analyses, a rational formation process
was proposed, as illustrated in Scheme 2. Owing to the pres-
ence of cellulose, hemicellulose, and lignin, the cornstalk bio-
mass was able to coordinate with metal ions through many
polar groups (i.e., OH and C=O), that is, [Fe(CN)6]4 ions
could coordinate with cornstalks to form a cornstalk-
[Fe(CN)6]4 composite material.[11–13] The [Fe(CN)6]4-cornstalk
composite could be pyrolyzed at a sufficiently high tempera-
ture, graphitized, and formed an Fe phase. Some carbon
atoms were incorporated into the Fe phase to form dense
Fe3C layers. By increasing carbonization temperature, the
active carbon atoms in the Fe3C layers could diffuse out to
form dense 2D carbon-atom layers (nanosheets) on the surfa-
ces of the formed planar “Fe-template” layers; any excess
amount carbon atoms were deposited on the formed nano-
sheets. During these processes, porous structures were formed
through the pyrolysis of groups in the cornstalk-
[Fe(CN)6]4composite. After the removal of Fe by using hydro-
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The galvanostatic charge–dis-

charge curves of electrode mate-
rials can be used to accurately
determine the specific capaci-
tance of supercapacitors in prac-
tical applications, which enable
their energy and power densities
to be calculated. Figure 6 a dis-
plays the galvanostatic charge–
discharge curves for the PGCS-
based and AC-1100 electrodes at
a current density of 1 A g1. All
of the obtained galvanostatic
charge–discharge curves were
highly linear and symmetrical, in-
dicating that the electrodes ex-
Scheme 2. The processes for the formation of PGCS. hibited excellent electrochemical
reversibility and charge–dis-

chloric acid treatment, PGCS were obtained. In this synthesis,

the K4[Fe(CN)6] catalyst was favorable to form a dense layer-
like “Fe template” that could limit the growth of the carbon
atoms along the 2D plane, similar to the planar Cu and Ni sub-
strates commonly used to prepare graphene by using CVD
methods.[37, 38]

Electrochemical performances
Good electron transportation and electrolyte penetration are
required properties for electrode materials used in EDLCs.[23–27]
For the synthesized PGCS, the porous structures were favora-
ble for the accessibility of the electrolyte and rapid ion diffu-
sion/transport. Both the 2D planar carbon nanosheets and the
graphitic structures could facilitate the fast transport of elec-
trons. Owing to its unique structure, PGCS were anticipated to
exhibit good performance as an electrode material for EDLCs.
The electrochemical performance of PGCS-based electrodes
was investigated in 6 m KOH electrolyte by using a three-elec-
trode system. Figure 5 shows the cyclic voltammetry (CV)
curves for the PGCS-based electrodes, which were tested at
scan rates of 10 and 100 mV s1. All of the PGCS-based electro-
des exhibited a relatively rectangular shape, indicating better
ion transport in the PGCS-based electrodes at high charge–dis-
charge rates and ideal capacitive behavior. The sample pre-
pared by directly pyrolyzing cornstalks under argon without Figure 5. CV curves for the PGCS-based electrodes in 6 m KOH solution at
any catalyst (denoted as AC-1100) was also studied. Different different scan rates: (a) 10 mV s1 and (b) 100 mV s1. The performance of the
AC-1100 sample prepared as that of the PGCS-1-1100 but without any cata-
from the PGCS electrodes, the AC-1100 electrode presented
lyst is also provided for comparison.
distorted CV curves. This was associated with the low SBET
value of 0.6 m2 g1 for AC-1100 (Figure S5), which implied
a nonporous structure that was not favorable for the rapid dif- charge properties.[40] The relationships between the physical
fusion of electrolyte ions. Also, the very broad and strong properties and the performance of all of the synthesized sam-
D band suggested an abundance of disordered carbon in ples are detailed in Table S3. The highest specific capacitance
AC-1100 (Figure S6),[39] implying poor electronic conductivity of 213 F g1 was demonstrated for the PGCS-1-1100 electrode,
that was not beneficial for fast electron transport. Therefore, al- and the lowest specific capacitance was demonstrated for the
though the typical quasi-rectangular characteristic was ob- AC-1100 electrode (only 49 F g1). All of the PGCS-based elec-
served in the CV curves, AC-1100 did not exhibit ideal perfor- trodes exhibited a much higher capacitance than that of the
mance because of a low SBET and poor electronic conductivity. AC-1100 electrode, demonstrating the importance of the

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Figure 6. (a) Galvanostatic charge–discharge curves for the PGCS-based and
AC-1100 electrodes at a current density of 1 A g1 in 6 m KOH electrolyte,
and (b) EIS spectra (presented as Nyquist plots) for the PGCS-based and
AC-1100 electrodes in 6 m KOH electrolyte (10 mHz to 100 kHz, AC ampli-
tude: 5 mV), and the corresponding electrical equivalent circuit that used to
fit the impedance spectra.
unique structure of the PGCS in EDLCs. The electrochemical
performances of the graphitic carbon nanocapsules structures
were also measured. The specific capacitances of the carbon
materials that contained graphitic carbon nanocapsules (de-
rived from different catalysts) were approximately 53–76 F g1
(see Figure S7 and Table S4 in the Supporting Information),
which were lower than the PGCS-based materials. The differ-
ence was attributed to the different carbon nanostructures.[40]
It was demonstrated that the structures of the PGCS could fa-
cilitate the rapid transport of the electrolyte and electrons,
leading to the improved electrochemical performance.
Electrochemical impedance spectroscopy (EIS) is an effective
method for studying the fundamental behavior of carbon ma-
terials in EDLCs. The EIS investigation was performed by using
an open-circuit voltage. The radius of the semicircle impe-
dance loop (as shown in Figure 6 b) in the high-frequency
region could be attributed to resistance associated with the
mass transfer/diffusion of ions through the porous structure of
carbon material.[41] PGCS-1-1100 exhibited the lowest resistance
to electrolyte transport, indicating that PGCS-1-1100 could pro-
vide a shortened path for electron transport and electrolyte
penetration. The straight line for the PGCS-1-1100 electrode in
the low-frequency region was closer to 908 compared to other
samples (vertical line for an ideal capacitor), further demon-
strating that the PGCS-1-1100 electrode could exhibit excellent
performance, which was consistent with the above charge–dis-
charge tests. Notably, compared to AC-1100, all of the PGCS-
based electrodes displayed a relatively small semicircle radius
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for the impedance loops at high-frequency and the straight
lines were closer to 908 at low-frequency, implying that the
structure of the PGCS was able to facilitate the rapid transport
of electrons and electrolyte penetration. The fitting equivalent
circuit model obtained by using the coupled nonlinear
Schrçdinger equation (CNLS) method is shown in Figure 6 b.
The entire capacitor circuit consisted of Rs, ZW, Rct, C, and Q.
Herein, Rs refers to the ionic conductivity of the electrolyte and
the electronic conductivity of the electrodes and current col-
lectors, which is the sum of the contact resistance and material
resistance.[42] ZW is the Warburg resistance, which is related to
ion diffusion/transport in the electrolyte.[43] Rct is the interface
resistance of ion adsorption–desorption on the electrode ma-
terials. C and Q are related to the capacitor layer that was
formed during the charge–discharge process. The fitting
results are listed in Table 2. The PGCS-1-1100 electrode exhibit-
Table 2. The calculated values of Rs, Rct, ZW, C, and Q through CNLS fitting
of the experimental impedance spectra based on the proposed equiva-
lent circuit displayed in Figure 6 b.[a]
Samples Rs [W] Rct [W] ZW [W] C [F] Q [F]
PGCS-05-1100 0.3861 0.5854 0.2708 2.3081 1.3594
PGCS-1-1000 0.3236 0.5663 0.1628 2.8657 1.6081
PGCS-1-1100 0.4319 0.6357 0.3226 1.2207 1.3223
PGCS-1-1200 0.5651 0.7531 0.5716 1.7852 1.2481
PGCS-3-1100 0.5077 0.6875 0.5343 2.567 1.1548
AC-1100 0.6916 0.9106 1.3529 0.8825 0.3205
[a] Calculated by using ZSimpWin software
ed the lowest Rs value of 0.3236 W, indicating that the
PGCS-1-1100 electrode had lower contact resistance and better
conductivity. Moreover, the AC-1100 electrode had the highest
Rs value of 0.6916 W. The results further demonstrated that the
graphitic nanosheet structure in the PGCS could enhance the
ability of rapid electron transport. It was concluded that the
PGCS-1-1100 and AC-1100 electrodes would exhibit the highest
and lowest performance in EDLCs, respectively.
The capacitance retention with current density is a crucial
criterion for estimating the potential application of carbon ma-
terials in EDLCs. An ideal EDLC should deliver the same energy
at any current density because of extremely fast ion transport,
which requires the carbon-based electrode material to exhibit
the following features: (i) only large mesopores (> 2 nm) in
carbon material, (ii) the diffusion path of electrolyte ions must
be reduced to a few nanometers, and (iii) the interactions be-
tween the electrolyte ions and the carbon surface are mini-
mal.[44, 45] Therefore, the power characteristics and the capaci-
tance retention should not obviously decrease with the in-
crease of current density. However, the ion “traffic jam” within
the micropores of electrode materials and the interaction of
the electrolyte with carbon functional groups increases Ohmic
resistance.[46] The electrode thickness is generally 10–300 mm,
resulting in the capacitance of EDLCs dramatically decreasing
at higher current densities.[36] Nevertheless, the samples con-
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sample was associated with its unique nanostructure, further

indicating its potential application for advanced electrodes in
high-performance supercapacitors.
Symmetric capacitors consisting of PGCS-1-1100 with aque-
ous and organic electrolytes were constructed, respectively.
6 m KOH aqueous solution and 1 m tetraethylammonium tetra-
fluoroborate in propylene carbonate (NEt4BF4-PC) were used as
the aqueous and organic electrolytes, respectively. As shown in
Figure 8 a and b, the symmetric triangular galvanostatic
charge–discharge curves indicated almost ideal capacitive be-
haviors with high coulombic efficiency at discharge current
densities of 0.5, 1, and 2 A g1 in both aqueous and organic

Figure 7. (a) Specific capacitance as a function of current density for PGCS-

based and AC-1100 electrodes in 6 m KOH solution, and (b) capacitance re-
tention and columbic efficiency of the PGCS-1-1100 electrode for
6000 cycles measured at a charge–discharge current density of 5 A g1
within the potential window 1.1–0.1 V in 6 m KOH solution. The inset in (b)
shows the galvanostatic charge–discharge curves of the last ten cycles of
the PGCS-1-1100 electrode after 6000 cycles.

taining PCGS exhibited good capacitance retention, and the re-

tained capacity of the samples was kept between 70.5 % to
81.3 % of the initial capacitance as the current density was in-
creased from 1 to 20 A g1 (Figure 7 a). The highest and lowest
capacitance retention was observed in the PGCS-1-1100 and
PGCS-05-1100 electrodes, respectively. Still, the AC-1100 exhib-
ited the poorest initial capacitance of 36.7 % when the current
density was increased from 1 to 20 A g1. Therefore, the
PGCS-1-1100 electrode exhibited the best performance owing
to its crystallinity, appropriate SBET value, and pore size.
The cycling stability of the electrode materials for supercapa-
citors is crucial for practical applications. Figure 7 b shows the
cycling lifetime tests over 6000 cycles for the PGCS-1-1100
sample at a current density of 5 A g1. PGCS-1-1100 exhibited
good cycling stability and 98 % of its initial capacitance was
maintained even after 6000 cycles, as demonstrated by the
charge–discharge curves for the last ten cycles (inset of Fig-
ure 7 b), which was crucial for its consideration in practical ap-
plications. Importantly, the columbic efficiency still remained
above 99 % after 6000 cycles. It was demonstrated that the re- Figure 8. Electrochemical performance of PGCS-1-1100 tested by using
petitive charge–discharge cycles did not result in any obvious a 2025-typr cell in aqueous and organic electrolytes at room temperature:
changes of the structure of PGCS-1-1100, and simultaneous ex- (a, b) the galvanostatic charge–discharge curves tested at different discharge
current densities (0.5–2 A g1) in 6 m KOH and 1 m NEt4BF4-PC electrolytes, re-
foliation of the electrode material (PGCS-1-1100) from the
spectively, and (c) Ragone plots obtained from the galvanostatic discharge
nickel foam current collector did not occur. The large capacity process at different current densities in 6 m KOH (0.5–50 A g1) and 1 m
and excellent cycling stability of the synthesized PGCS-1-1100 NEt4BF4-PC (0.5–30 A g1), respectively.

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electrolytes. The specific capacitances (Ccell) for both cells were
about 63.5 and 47.3 F g1 at the current density of 1 A g1 in
6 m KOH and 1 m NEt4BF4-PC electrolytes, respectively. A higher
specific capacitance is generally obtained by using aqueous
electrolytes compared to organic electrolytes. Nevertheless,
one of the main advantages of EDLCs with organic electrolytes
is that it is possible to deliver a higher energy density over
a wider voltage window.[47] Further characterizations were
demonstrated in the Ragone plots, as shown in Figure 8 c.
A specific energy density of up to 9.4 Wh kg1 could be
achieved at extremely low power densities, and 8.3 Wh kg1
was retained at a power density of 10.5 kW kg1 in 6 m KOH
electrolyte. Additionally, a specific energy density of
61.3 Wh kg1 was delivered at a low power density in 1 m
NEt4BF4-PC electrolyte. Moreover, a high specific energy density
of 40.6 Wh kg1 could be retained, even at a higher power den-
sity of 10.5 kW kg1. The performances in both aqueous and or-
ganic electrolytes were much greater than that of the previ-
ously reported porous carbon-based materials, such as porous
graphitic carbon, activated carbon/graphene, and carbon
sphere/graphene composites.[48–50] The good performance of
PGCS-1-1100 in both aqueous and organic electrolytes further
highlighted its potential in high-performance supercapacitors.
Conclusions
We demonstrate an in situ, self-generating template strategy,
based on the carburized effect of iron from cornstalks, for the
synthesis of PGCS. The SBET and crystallinity of the synthesized
PGCS can be tuned by changing the experimental parameters,
including the catalyst concentration and carbonization temper-
ature. The nanostructures of the obtained PGCS exhibit excel-
lent energy storage performance as candidates for advanced
electrode materials for supercapacitors. Remarkably, the syn-
thesized PGCS-1-1100 material exhibits good capacitive charac-
teristics (higher specific capacitance, improved capacity reten-
tion, as well as higher rate capability and cycling stability) in
6 m KOH electrolyte. Also, the symmetrical capacitors can deliv-
er high energy and power densities in both aqueous and or-
ganic electrolytes. The excellent performance is attributed to
the unique structure of the PGCS: (i) the porous structure in
the PGCS is favorable for the rapid diffusion of electrolyte ions
by providing low-resistant pathways, and (ii) owing to the
nature of excellent conductivity, the planar and graphitic struc-
tures of the PGCS can facilitate the electron transport. Addi-
tionally, the synthetic strategy opens up a new path to synthe-
size PGCS for applications in energy storage. Most importantly,
this study emphasizes the exploration and adoption of the
most abundant resource available in nature, that is, cornstalks,
in the field of materials science.
Experimental Section
Preparation of PGCS
In a typical synthesis, cornstalks (2.6 g) without further treatment
were immersed into K4[Fe(CN)6] aqueous solution (180 mL, 0.1 m)
 2013 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
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at 35 8C for 4 h. During this process, the cornstalks coordinated
with [Fe(CN)6]4 to form a cornstalk-[Fe(CN)6]4 composite. Then,
the solid was collected and a pyrolytic procedure was conducted
at 1100 8C for 2 h with a constant heating rate of 5 8C min1 in an
argon atmosphere. Subsequently, the sample was treated with hy-
drochloric acid (120 mL 1.0 m) at 85 8C for 6 h. Finally, the PGCS
were obtained after being washed with water until neutralized and
dried in an 80 8C oven. The resultant samples were denoted as
PGCS-c-T, where c was the concentration of the K4[Fe(CN)6] solution
and T was the carbonization temperature. Therefore, the above
synthesized sample was named as PGCS-1-1100. To study the effect
of the carbonization temperature on the performance of the resul-
tant PGCS, different carbonization temperatures were used to pre-
pare PGCS-1-1000 (1000 8C) and PGCS-1-1200 (1200 8C). Samples
synthesized from different concentrations of K4[Fe(CN)6] catalyst
were also studied, denoted as PGCS-05-1100 (0.05 m) and
PGCS-3-1100 (0.3 m). For comparison, a sample was prepared under
the same conditions as that of the PGCS-1-1100 but without any
catalyst; this sample was denoted as AC-1100. To study the effect
of different metal catalysts on the nanostructure of the resultant
carbon materials, the synthesis was performed by replacing
K4[Fe(CN)6] with FeCl2, CoCl2, and NiCl2 (180 mL, 0.1 m in all cases);
the cornstalks coordinated with the Fe2 + , Co2 + , and Ni2 + ions to
form cornstalk-Fe2 + , cornstalk-Co2 + and cornstalk-Ni2 + composites,
respectively. After carbonization at 1100 8C and subsequent remov-
al of the catalyst by using hydrochloric acid, the graphitic carbons,
denoted as GC-FeCl2-1100, GC-CoCl2-1100, and GC-NiCl2-1100, were
obtained. The sample numbers and detailed experimental parame-
ters are displayed in Table S1.
Characterizations
XRD patterns were obtained by using a Rigaku D/max-IIIB diffrac-
tometer with CuKa (l = 1.5406 ) radiation. The accelerating volt-
age and the applied current were 40 kV and 20 mA, respectively.
TEM images were obtained with a JEM-2100 electron microscope
(JEOL) and an acceleration voltage of 200 kV. Carbon-coated
copper grids were used as the sample holders. Raman measure-
ments were performed with a Jobin Yvon HR 800 micro-Raman
spectrometer at 457.9 nm. X-ray photoelectron spectroscopy (XPS)
studies were performed on a Kratos-AXIS UL TRA DLD with an AlKa
radiation source. The N2 adsorption–desorption isotherms of the
samples were obtained by using a Micromeritics TriStar II. The sam-
ples were outgassed for 14 h at 210 8C under vacuum before the
measurements were obtained. The PSD was calculated by using
the NLDFT method.
Electrode preparation and electrochemical measurements
The working electrodes were prepared by mixing the prepared
PGCS active materials (75 wt %), carbon black (20 wt %), and poly-
tetrafluoroethylene (PTFE; 5 wt %). The above electrode material
mixture (5 mg) was pressed onto a foam nickel electrode. The elec-
trochemical performance was tested by using a three-electrode
system in 6 m KOH aqueous electrolyte at room temperature. A sa-
turated calomel electrode (SCE) and Pt slice were used as the refer-
ence and counter electrodes, respectively. CV curves were obtained
by using a BAS100B electrochemical workstation. The constant-cur-
rent charge–discharge capacitance tests (voltages window:
1.1–0.1 V) were conducted on a CHI 660D electrochemical work-
station. The capacitance was calculated by using the following
formula:[51]
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C ¼ IDt=ðmDVÞ ð1Þ
herein C is the capacitance (F g1), I and Dt are the constant dis-
charge current (A) and the discharge time (s), respectively, and m
and DV are the mass of active material within the electrode (g) and
the potential range (V), respectively. The columbic efficiency was
calculated by using the following formula:[52]
h ¼ td =t c ð2Þ
herein tc and td represent the times of charge and discharge, re-
spectively. The two-electrode cells were prepared by using 2025-
type coin cells. The aqueous and organic electrolytes used were
KOH solution (6 m) and NEt4BF4-PC (1 m), respectively. The symmet-
ric cells were charged and discharged by using a LAND battery
tester. The specific capacitance as well as power and energy densi-
ties were calculated based on the total mass of the anode and
cathode materials.[48] The energy densities (Ecell) were calculated by
using the following formula:
E cell ¼ 0:5 C cell V 2 ð3Þ
herein Ccell and V are the total cell capacitance and the cell opera-
tion potential, respectively. The power density (Pcell) was calculated
according to the following formula:
Pcell ¼ V 2 =ð4 ESR mÞ ð4Þ
herein ESR is the equivalent series resistance and m (g) is the total
mass of anode and cathode materials.
Acknowledgements
We gratefully acknowledge the support of the Key Program Proj-
ects of the National Natural Science Foundation of China (no.
21031001), the National Natural Science Foundation of China
(nos. 20971040, 91122018, 21101060, 21101061), the Cultivation
Fund of the Key Scientific and Technical Innovation Project, Minis-
try of Education of China (no. 708029), and Specialized Research
Fund for the Doctoral Program of Higher Education of China
(nos. 20112301110001, 20112301110002).
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Fields of gold? Porous graphitic carbon
nanosheets (PGCS) have been synthe-
sized by a self-generating template
strategy based on the carburized effect
of iron with cornstalks. The synthesized
 2013 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
L. Wang, G. Mu, C. Tian, L. Sun, W. Zhou,
P. Yu, J. Yin, H. Fu*
&& – &&
Porous Graphitic Carbon Nanosheets
Derived from Cornstalk Biomass for
Advanced Supercapacitors
PGCS exhibit excellent capacitive perfor-
mance owing to their unique porous
nanostructures and graphitic carbon
nanosheets, which can facilitate ion and
electron transport, respectively.
ChemSusChem 0000, 00, 1 – 11 &11&
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