Article BULLETIN OF THE

DOI: 10.1002/bkcs.12145 S. Hong et al. KOREAN CHEMICAL SOCIETY

Hierarchical Porous Carbon Materials Prepared by Direct

Carbonization of Metal–Organic Frameworks as an Electrode Material
for Supercapacitors
Soonsang Hong,† Younghoon Kim,† Yelin Kim,‡ Kyungwon Suh,† Minyoung Yoon,§,* and
Kimoon Kim†,‡,*
†
Center for Self-assembly and Complexity, Institute for Basic Science, Pohang 37673, Republic of Korea
‡
Department of Chemistry and Division of Advanced Materials Science, Pohang University of Science
and Technology, Pohang 37673, Republic of Korea. *E-mail: kkim@postech.ac.kr
§
Department of Chemistry and Green-Nano Materials Research Center, Kyungpook National University,
Daegu 41566, Republic of Korea. *E-mail: myyoon@knu.ac.kr
Received September 7, 2020, Accepted October 30, 2020, Published online November 10, 2020

We report the synthesis and characterization of hierarchical porous carbons (HPCs) prepared by direct car-
bonization of zinc-based metal–organic frameworks (MOFs), and their electrochemical performance as an
electrode material for supercapacitors. All the HPCs showed high porosity (Brunauer–Emmett–Teller
(BET) surface areas 1000–1820 m2/g) with micro-, meso-, and macropores. The HPC-based electrodes
exhibited a high-specific capacitance in the range of 164–203 F/g (scan rate: 10 mV/s), which suggests
that these porous carbons may be useful for fabricating supercapacitors. Among the HPCs, HPC-4 with
the largest surface area as well as with ~1% nitrogen content exhibited the highest specific capacitance,
which is comparable with those of other reported carbon materials. This work suggests that the hierarchi-
cal porosity and nitrogen doping in HPCs may enhance their conductivity and specific capacitance.
Keywords: Porous carbon, Metal–organic framework, Hierarchical porosity, Supercapacitor, N-doping

Introduction applications such as supercapacitors.13-15 Compared to the

In recent years, porous carbon materials exhibiting large
surface area, high conductivity, and high electrochemical
stability have been widely employed in electrochemistry
fields such as supercapacitors, electrocatalysis, and lithium-
ion batteries.1,2 So far, various synthetic strategies have
been utilized for the fabrication of carbon materials, includ-
ing carbonization/activation, laser ablation, chemical or
physical activation methods, and template-assisted carboni-
zation.3 Among the strategies aforementioned, the
template-assisted carbonization method has many advan-
tages including fine-tuning of the morphology, uniform
pore size distribution (PSD), and functionalization.4-7 For
instance, zeolite, silica, and zinc oxide have been used as a
template, providing well-defined pore structures and
narrow-size distributions. The template-assisted methods,
however, require extra carbon source to generate a carbon
framework and the template materials should be removed
by specific solvent and acid afterwards.
Metal–organic frameworks (MOFs) which possess highly
ordered structures and large pores, have also been explored
for template casting methods regarding the preparation of
porous carbons.8-13 Notably, carbonization using a MOF
precursor as a template as well as a carbon source can con-
siderably enhance the stability and conductivity of resulting
carbon materials which may be useful in electrochemical
conventional methods, the MOF-derived synthetic strategy
has several benefits in the fabrication of porous carbon
materials: (1) it is possible to synthesize the materials with
inherent diversity providing precise control over porosity,
(2) in contrary to inorganic templates, MOFs contain
organic ligands in the frameworks and therefore require no
additional carbon source at least in principle, and (3) direct
carbonization of MOFs with nitrogen-containing moieties
may allow the formation of nitrogen-doped porous carbons,
which can improve the electrochemical properties of the
materials. Therefore, the use of MOFs as templates is one
of the efficient ways to prepare porous carbon materials for
electrochemical applications.
In 2012, we reported the synthesis of a series of porous
carbon materials by direct carbonization of MOF materials
and the strong correlation between the Zn/carbon ratio of
the starting materials and the Brunauer–Emmett–Teller
(BET) surface area of the resulting carbon materials.16 By
virtue of the hierarchical porosity, high stability, and con-
ductivity of the carbonized materials, we envisioned that
they can be utilized as promising materials for super-
capacitors. Herein, we report the preparation of hierarchical
porous carbons (HPCs) by direct carbonization of zinc con-
taining MOFs and their electrochemical properties as an
electrode material for supercapacitors. The electrochemical
performance of the HPCs was investigated by cyclic

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Article
ISSN (Print) 0253-2964 | (Online) 1229-5949
voltammetry (CV) and galvanostatic charge/discharge
(GCD) measurements. The HPC-based electrodes exhibited
a rectangular CV curve with a high-specific capacitance in
the range of 164–203 F/g (scan rate: 10 mV/s), which is
comparable with those of reported high-performance carbon
materials. Our work suggests that a large surface area with
hierarchical porosity and nitrogen doping in HPCs are
importance in achieving high conductivity and specific
capacitance.
Experimental
Preparation of HPCs. Zinc-containing MOF precursors,
[Zn4O(bdc)3] (1),17 [Zn2(bdc)2(dabco)] (2),18 [Zn2(bdc)
(L-lac)(DMF)] (3),19 and [Zn3(fumarate)3(DMF)2] (4)16
were prepared according to the literature. HPC materials
HPC 1–HPC-4, were synthesized by direct carbonization
of MOFs 1–4, respectively, without an additional carbon
source, following the previously reported procedure.16
More specifically, the MOF precursors were thoroughly
washed with fresh DMF and dried under dynamic vacuum.
The dried MOFs (~1.00 g) were transferred to an alumina
container and placed in a quartz tube equipped furnace with
a gas flowing system. They were carbonized at 1100
C
(heating rate: 10
C/min) with flowing of inert gas (Ar, flow
rate = 200 mL/min) for 8 h. The tube furnace was cooled
down to ambient temperature. The resulting carbon pow-
ders (HPC-1 to 4, respectively) were collected (~100 mg).
As-synthesized carbon materials were used for characteriza-
tion and electrochemical property measurements without
further treatment.
Characterization. The powder X-ray diffraction (PXRD)
profiles were obtained on a Bruker D8 Advance (Bruker,
Germany) equipped with a Cu sealed tube (λ = 1.54 Å)
with 40 kV and 40 mA of X-ray generator parameter. The
data were collected using following conditions incre-
ment = 0.05
and scan speed = 3 deg./min. N2 sorption iso-
therms were measured using a volumetric adsorption
apparatus, Quantachrome Autosorb 1MP (sample activation
condition: 150
C for 8 h). A high purity gas was used for
all gas sorption experiments (N2: 99.999%, Linde Korea).
BET surface area of HPCs material was calculated in a
P/P0 range of 0.05–0.10. PSDs and cumulative pore vol-
umes were calculated using the nonlocal density functional
theory (NL-DFT) model with cylindrical pore geometry of
carbon adsorbent; the NL-DFT method is an integral part
of the Quantachrome Autosorb 1MP instrument (Quan-
tachrome, USA). C, H, N elemental analyses (EA) data
were obtained using a VarioMICRO (Elementar, Germany).
X-ray photoemission spectroscopy (XPS) data were col-
lected with a K-Alpha ESKA SYSTEM (Thermo Scientific,
USA) equipped with a monochromatic Al-Kα (1486.8 eV)
X-ray source (power: 225 W). The survey spectra
(0–1200 eV) and the high-resolution spectra of the C 1 s, O
1 s, N 1 s, Zn 2p regions were obtained at analyzer pass
energies of 50 eV and 20 eV, respectively. The step
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BULLETIN OF THE
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energies of 1.0 eV and 0.1 eV were used for survey spectra
and high-resolution spectra, respectively. The X-ray beam
focusing area for XPS analysis was circular shaped with
~1.1 mm of a diameter.
Preparation of Electrodes Using HPCs and Measure-
ment of Their Electrochemical Properties. The electro-
chemical properties were obtained using a symmetric
two-electrode cell (capacitor) with the HPC material as an
electrode (~1.0 mg of HPCs for each electrode without any
additives), 1.0 M H2SO4 aqueous solution as an electrolyte,
where a glassy paper was used as a separator (apparent
electrode area of 0.38 cm2). The separator soaked in the
electrolyte solution was sandwiched between two HPC
materials. Pt plates were employed as a charge collector for
each electrode. Two symmetric HPC electrodes acted as
cathode and anode in the supercapacitor configuration. The
capacitor cell was soaked in 1 M H2SO4 electrolyte solu-
tion for 60 min before capacitance measurement.
All the electrochemical measurements were carried out at
room temperature under air atmosphere. The specific capac-
itance of the cells was studied using CV and GCD mea-
surement. Cyclic voltammograms (CV) were recorded
using an electrochemical workstation (SP-300, BioLogic,
France) at various sweep rates (−0.50 to 0.50 V) for the
capacitors. GCD experiments at different current densities
(−0.50 to 0.50 V) were carried out using the same
instrument.
Following Eq. (1) was used for the calculation of the
specific capacitance:
C = 2 × ΔQ=ðΔV × mÞ ð1Þ
where ΔQ is the charge integrated from a specific voltage
range ΔV, and m is the weight of the electrode material.
Following Eq. (2) was used to calculate the specific
capacitance of the individual electrode:
C = 2 × I × Δt=ðΔV × mÞ ð2Þ
where I is the discharge current, Δt is the discharge time
from 0 to −0.4 V, ΔV is the voltage difference within the
discharge time Δt, and m is the weight of the electrode
material. The total capacitance that can be obtained from
the sum of symmetric two electrode capacitors, which gives
the factor of two in these equations.
Results and Discussion
Synthesis and Characterization of HPCs. Four HPC
materials (HPC-1 to HPC-4) were synthesized by direct
carbonization of the zinc containing MOF precursors 1–4,
respectively, at 1100
C.16 The chemical composition of the
resulting HPCs was established by EA and XPS (Table S1
and Figure 1). Although some porous carbons prepared
from MOFs use additional carbon sources such as furfuryl
alcohol,8,20 this synthetic strategy does not require
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Article Hierarchical Porous Carbon Materials
additional carbon source similar to the recent porous carbon
synthesis using MOFs.21,22 During the carbonization pro-
cess, zinc ions are reduced to zinc metal by carbon material
and evaporated at 1100
C because of the low boiling point
of metallic zinc (907
C). However, a small portion of oxy-
gen and nitrogen atoms can remain when the MOF precur-
sors contain nitrogen atoms in the ligands. For example,
elemental analysis showed that HPC-1 and HPC-3 pre-
pared from nitrogen free MOF precursors, 1 and 3, pro-
duced nitrogen free porous carbon, whereas the MOFs
comprising nitrogen containing ligands, 2 and 4, produced
nitrogen doped porous carbons, HPC-2 and HPC-4 that
Figure 1. XPS data of (a) HPC-1, (b) HPC-2, (c) HPC-3, and
(d) HPC-4.
Figure 2. Cyclic voltammograms at different sweep rates (10–100 mV/s) for HPCs: (a) HPC-1, (b) HPC-2, (c) HPC-3, and (d) HPC-4.
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each contain ~1% nitrogen. The presence of nitrogen was
also confirmed by XPS analysis (Figure 1). Only HPC-2
and HPC-4 showed a peak corresponding to N 1s in XPS
data. The PXRD profiles of the HPCs showed their amor-
phous nature (Figure S1, Supporting Information), as
reported previously.16
Porosity Analysis of Hierarchical Porous Carbons. The
overall N2 sorption isotherms (Figure S2) of the four HPCs
are almost the same as reported previously.16 In this study,
however, we decided to investigate the porosity of the
HPCs in more detail as it may be important in understand-
ing their electrochemical behavior. The N2 sorption iso-
therm of HPCs showed the combined characteristics of
type I/II/IV isotherms. A steep initial uptake was observed
at low pressures (type I), followed by a slope at the inter-
mediate pressure accompanied by a hysteresis behavior
(type IV) during desorption. At high pressures, the N2 iso-
therm drastically increased (type II), suggesting the com-
bined effects of hierarchical pores in the HPCs including
micropores, mesopores, and macropores.
The PSD and cumulative pore volumes were estimated
using NLDFT and summarized in Table S2.23 PSD of the
four HPCs are shown in Figure S3a. The PSD demon-
strated both micro- and mesopores exist in all HPCs. The
cumulative pore volume of representative materials is
shown in Figure S3b. HPC-2 has a small pore volume,
whereas HPC-4 has a large pore volume, which may affect
the specific capacitance of the carbon electrode.24
Electrochemical Properties of HPCs as an Electrode
Material of Supercapacitors. An electrochemical
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capacitor (supercapacitor) stores electrons (charge) in the
double layers of porous carbon electrodes surface by elec-
trostatic interactions. The separation of charged species
allows the electric energy (electron) storage across the
electrode-electrolyte interface. Therefore, large surface area
of electrode material, conductivity of electrode materials,
and interaction between electrode and electrolyte is critical
factors for the determination of capacitance of a super-
capacitor. In general, the specific capacitance of a super-
capacitor is linearly proportional to the specific surface area
of electrode materials. (C = eS/d, where e is the permittivity
of the electrolyte, S is the surface area of the electrode-
electrolyte interface, and d is the distance between the
electrode surface and the solvated ions).25,26 Especially, a
hierarchical porous structure is beneficial for high capaci-
tance because it enhances electrochemical accessibility of
the solvated ions allowing facile charging and discharging
of the supercapacitor. Besides, the specific capacitance is
affected by surface property of the materials including
conductivity.27
The electrochemical properties of HPCs were investi-
gated with CV using two-electrode HPC-based capacitors
cycling (−0.5 to 0.5 V) at various sweep rates. It should be
noted that the electrode was made of only the HPCs with-
out the addition of any binders and conductive reagents.
The specific capacitances at various sweep rates of four

Table 1. Specific capacitance of HPCs and reported MOF-derived porous carbon materials in the literature.
BET surface area Sweep rate Current density Specific capacitance Specific capacitance
Samples (m2/g) (mV/s) (mA/g) (F/g) (F/cm2)
HPC-1 1454 10 100 164a/182b 426a/472b
HPC-2 987 10 100 180a/221b 468a/574b
HPC-3 1714 10 100 166a/198b 431a/514b
HPC-4 1834 10 100 203a/230b 527a/598b
NPC8 2872 5 250 204a/258b —
GNRib32 1492 10 100 193a/189b —
S-90033 1823 5 100 219a/53.8b 92.0a/22.6b
MWCNT/NPC-L34 928 5 200 293a/219b —
CIRMOF-3-95035 553 5 100 239a/166b —
a
Specific capacitance calculated from cyclicvoltammetric measurements.
b
Specific capacitance calculated from galvanostatic charge/discharge (GCD) measurements.

Figure 3. Galvanostatic charge/discharge curves at different current densities for HPCs: (a) HPC-1, (b) HPC-2, (c) HPC-3, and
(d) HPC-4.

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Article Hierarchical Porous Carbon Materials
capacitors are presented in Figure 2 and summarized in
Table 1. The specific capacitance of four supercapacitors
comprising HPCs showed 10–20% difference when the
sweep rate was changed from 10 to 100 mV/s, which is
characteristic for supercapacitors comprising hierarchical
pores. The difference may be due to the diffusion limitation
of solvated ions to the micropores of HPCs. However, the
CV of all the capacitors showed almost perfect rectangular
shape at various sweep rates demonstrating an ideal capaci-
tor behavior. All the HPCs showed the highest specific
capacitance with a scan rate of 10 mV/s, which was in a
range of 164–203 F/g. The resulting capacitance of the
HPCs is quite comparable with other high-performance
porous carbon materials reported in the literature (Table 1).
The surface area and pore volume of HPCs are the
important criteria in the field of supercapacitors.9 In this
work, the HPCs showed a reasonable correlation between
the capacitance and surface area. In particular, the super-
capacitor made of HPC-4 which has the largest BET sur-
face area among the HCPs, showed the highest specific
capacitance at any scan rate. Note that despite the similar
BET surface area, HPC-4 with ~1% N content showed
much higher specific capacitance (174–203 F/g) than that
of HPC-3 (156–166 F/g) with no N content. Moreover,
although HPC-2 with a residual N content showed a lower
BET surface area than HPC-1 with no N, the specific
capacitance of the former (163–180 F/g) was higher than
that of the latter (144–164 F/g), which indicated a positive
effect of nitrogen doping on the specific capacitance.
Taken together, these results suggested that the high elec-
trochemical performance of the HPCs were benefited by
the presence of both a hierarchical pore structure and
residual nitrogen content, which is consistent with other
studies. 28–31
GCD measurements between −0.5 and 0.5 V have also
been carried out to assess the electrochemical performance
of the HPCs as a promising electrode material for super-
capacitor (Figure 3). The specific capacitances of the HPCs
at various current densities are shown in Table 1 and S3.
No voltage drop was observed at the beginning of the dis-
charge process and all the samples exhibited nearly triangu-
lar shapes at the current densities. The feature indicates a
high columbic efficiency and ideal capacitor behavior, con-
sistent with the results of voltammetric studies. In particu-
lar, HPC-4 showed the highest specific capacitance of
230 F/g at a current density of 100 mA/g. Once again, the
excellent performance of the HPC is presumably due to its
high surface area as well as nitrogen doping.
Conclusion
In summary, we have synthesized and characterized new
HPC materials by direct carbonization of MOFs and
investigated their electrochemical performance as a prom-
ising electrode material for supercapacitors. Among the
HCPs, those derived from nitrogen-containing MOF
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precursors showed ~1% nitrogen content. All the HPCs
showed a high surface area with micro-, meso-, and
macropores. While all the HPCs showed high-specific
capacitance values, in particular, HPC-4 with the largest
surface area as well as with ~1% nitrogen content
exhibited the highest specific capacitance, which is com-
parable with those of other reported high-performance car-
bon materials. These results therefore suggest that a large
surface area with hierarchical porosity and nitrogen dop-
ing in HPCs are importance in achieving high conductiv-
ity and specific capacitance. For a better understanding of
the relationship between the porosity and amount of
N-doping in HPCs and their electrochemical performance,
however, a systematic study is further required. Neverthe-
less, this work may provide a useful clue to design and
synthesize better carbon materials suitable for fabricating
supercapacitor electrodes
Acknowledgments. We thank C. Jo and J. Lee for helpful
discussions. This work was supported by the Institute for
Basic Science (IBS) [IBS-R007-D1].
Conflict of interest. The authors declare no conflict of
interest.
Supporting Information. Additional supporting informa-
tion may be found online in the Supporting Information
section at the end of the article.
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