Applied Surface Science 487 (2019) 189–197

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Applied Surface Science

journal homepage: www.elsevier.com/locate/apsusc

Full length article

Tea waste derived microporous active carbon with enhanced double-layer T

supercapacitor behaviors
⁎
Xinyu Songa, Xinlong Mab, Yun Lib, Liang Dinga, Ruiyu Jianga,
a
Key Laboratory for Advanced Technology in Environmental Protection of Jiangsu Province, Yancheng Institute of Technology, Yancheng 224051, PR China
b
State Key Laboratory of Heavy Oil Processing, China University of Petroleum, Beijing, Changping 102249, China

A R T I C LE I N FO A B S T R A C T

Keywords: Activated carbon (TC1200) is prepared from tea waste via activation and carbonization. The specific surface area
Biomass of TC1200 is 911.92 m2 g−1 and N-doping is achieved simultaneously due to the existence of N-enriched
Active carbon components in the carbon precursor. The TC1200 exhibits superior capacitive performances on a symmetric
Electrical conductivity supercapacitor in the aspects of ultralong cycle stability (96.66% capacitance retention after 16,000 cycles at
Hydrophilicity
4 A g−1) and ultrahigh power density (33,494.70 W kg−1 for an energy density of 19.45 Wh kg−1). The en-
Supercapacitor
hanced electroconductivity and the excellent wettability provided by the N elements synergistically facilitate the
diffusion of the electrolyte ion into the bulk of the carbon material, greatly contributed to the double-layer
capacitive behavior and the capacitance of the carbon material. This methodology supports the high-value added
utilization of the biomass and provides an opportunity for the scalable production of activated carbons for
supercapacitor energy storage devices.

1. Introduction environmentally friendly, sustainable and renewable carbon resources.

As the environmental protection has been arousing public attention,
the countries worldwide are replacing the traditional fossil fuel with
green energy resources such as solar energy, wind energy and electric
energies [1]. The electrochemical energy storage elements such as su-
percapacitors [2], lithium ion batteries [3–4], sodium ion batteries [5],
Li-S batteries [6–7] and lithium ion capacitors (LIC) [8–9] have been
researched extensively. To meet the urgent requirements for the high
power electrochemical energy storage devices, supercapacitors are the
most feasible option due to their fast charge-discharge performance,
long cyclability and high powered density [10–11]. The most ex-
tensively researched electrode materials for supercapacitors are gra-
phene and activated carbons (ACs). Graphene has less industrial ap-
plications compared with ACs, because of the high cost and the
restacking of the thin graphite layers. ACs are considered to be the most
promising materials as commercial electrodes of supercapacitors due to
the rich pore channels and the high specific surface area which may
greatly contribute to the high specific capacities [12]. ACs are mainly
synthesized via the pyrolysis and activation of carbon precursors in-
cluding fossil fuels, biomass or their derivatives [13–16]. Nowadays,
various biomass such as coconut shells [17], bamboo [18], corn grain
[19], straw [20] and some organic wastes [21] are widely explored due
to their abundant, economic advantages, moreover, they are
Tea waste, which is a daily waste residue that plentifully generated
after extraction all over the world, often be discarded directly. The
cellulose, hemicelluloses, lignin and polyphenol constitute 70–80% of
the tea waste [22], and the protein is another important constituent
which is rich in nitrogen-containing compounds. The aforementioned
characteristics endow the tea waste with great potential to be used as
carbon precursor for high-performance electrode materials.
Researchers usually concentrate on the pore channels of the carbon
materials to ensure the ion diffusion and shorten the pathways [23–24],
however, the poor electric conductivity and the poor wettability are the
long-standing unsolved issues which limit the application on the hybrid
electric devices. Herein, an activated carbon with superior super-
capacitor performance has been prepared by engaging tea leaves as
carbon precursor. The as-prepared carbon possesses both good elec-
trical conductivity and excellent wettability, which greatly contributes
to the rate performance and long cyclability. The strategy facilitates
access to high quality ACs that applicable to supercapacitors and pro-
vides an opportunity for the high value-added utilization of the waste
residue from daily life.

⁎
Corresponding author.
E-mail address: jiangry@ycit.edu.cn (R. Jiang).

https://doi.org/10.1016/j.apsusc.2019.04.277
Received 23 February 2019; Received in revised form 12 April 2019; Accepted 30 April 2019
Available online 01 May 2019
0169-4332/ © 2019 Elsevier B.V. All rights reserved.
X. Song, et al.
Scheme 1. Schematic illustration of the preparation of TC1200.
2. Experimental section
2.1. Synthesis process
Tea leaves were boiled in deionized water for 10 min for further
purification. Tea powder was obtained after dried and crushed with a
mini-type pulverizer. KOH was used as active agent with the KOH to tea
powder mass ratio of 2. The mixture of KOH and tea powder was cal-
cined at 900 °C for 60 min in a horizontal tube furnace with the pro-
tection of argon. After cooling to room temperature, the powder was
purified by diluted hydrochloric acid washing to remove the potassium
compounds, and the carbon obtained was named as TC. The TC was
treated at 1200 °C for further calcination, and the final carbon was la-
beled TC1200. A commercial coaly AC provided by Chamboard
Petrochemical Co., Ltd. was used for comparison without further pur-
ification.
2.2. Characterization
The as-prepared materials were characterized by transmission
electron microscopy (TEM, JEM 2100, JEOL) equipped with energy
dispersive spectroscopy (EDS) elemental mapping devices, scanning
electron microscopy (SEM, Quanta 200F, FEI, Holland), atomic force
microscope (AFM, SPM-9600), Raman spectroscopy (Renishaw
RM2000, at 633 nm). Specific surface area (SSA) was measured on
Micromeritics ASAP 2020 and was calculated using Brunauer-Emmett-
Teller (BET) adsorption model. The pore properties were derived from
the adsorption branch of the isotherms, calculated using the
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Applied Surface Science 487 (2019) 189–197
Barrett–Joyner–Halenda (BJH) method. Contact angel was tested on
optical contact angel & interface tension meter (SL200KS, KINO, USA).
2.3. Electrochemical measurements
The carbon materials (TC or TC1200) were stirred into a slurry
using N-methyl-2-pyrrolidinone as solvent, containing 70% TC or
TC1200, 10% carbon black and 20% LA133 as binding agent. Nickel
foam and stainless-steel wire mesh (1 cm2) were used as current col-
lector in 1 M KOH electrolyte (voltage range 0–1 V) and 1 M Na2SO4
electrolyte (voltage range 0–1.6 V) respectively. The mass loading was
kept at around 2 mg cm−2 for all the electrodes. Considering that the
two-electrode supercapacitor test can better reflect the real working
conditions than the three-electrode test in actual applications, sym-
metric supercapacitor was fabricated in the form of button cell battery.
The related tests were performed on the CHI660D electrochemical
workstation.
To investigate the capacitive behavior, the specific capacitance was
calculated using Eq. (1) [25] according to the profiles from chron-
opotentiometry measurement.
∆V ⎞
Csp = 2 × I / m ⎛
⎝ ∆t ⎠ (1)
The energy and power densities of the electrodes are evaluated from
the GCD profiles using the Eqs. (2) and (3) [26], respectively:
1 1000
E= Csp (∆V )2 ×
2 3600 (2)
X. Song, et al. Applied Surface Science 487 (2019) 189–197

Fig. 1. The SEM of TC (a) and TC1200 (b); the TEM picture of TC1200 (c) and high resolution (d); the AFM picture and height profiles of TC1200 (e).

191
X. Song, et al. Applied Surface Science 487 (2019) 189–197

Fig. 2. The N2 adsorption-desorption isotherm of AC, TC and TC1200 (a) and the pore size distribution (b); Raman spectra of TC1200 (c) and the value of ID/IG band
ratios of AC, TC and TC1200 (d). The XPS spectrum of TC1200 (e) and the high resolution spectra of C (f) and N (g).

192
X. Song, et al.
Fig. 3. The CV curves of AC (a), TC (b), and TC1200 (c and d).
E mesopore (Fig. 2b), the same as commercial AC. The DG peak of Raman
P=
∆t /3600 (3)
where Csp is the specific capacitance (F g−1), I is the discharge current
(A) and m is the mass loading of individual electrode (g). ΔV and Δt are
potential window (IR drop corrected) (V) and discharge time (s) re-
spectively in the discharge process. E is the average energy density of
the electrode (Wh kg−1), P is the average power density of the electrode
(W kg−1).
3. Results and discussion
The synthesis process of TC1200 is depicted in Scheme 1. The
carbon-rich components and protein rearrange into amorphous carbon
after cracking and polycondensation during the calcination process. In
this step, TC with abundant micropores is generated with KOH as ac-
tivator agent. TC1200 is obtained after further carbonization of TC at
1200 °C, and the final carbon was labeled as TC1200. As shown in the
SEM picture, both TC (Fig. 1a) and TC1200 (Fig. 1b) demonstrate the
typical porous morphology of AC (Fig. S1), and the 1200 °C calcination
does not destroy the structure of TC. The TC1200 has uniform and thin
carbon layers with homogeneously distributed micropores (Fig. 1c and
d), which is confirmed by the AFM characterization. The height of the
two cross sections are highly consistent at around 5 nm (as shown in
Fig. 1e), indicating the fairly uniform height of the TC1200 (around 10
graphite layers), which can be attributed to the plane network config-
uration of the original tea leaves.
Porosity is a pretty important factor for the supercapacitor beha-
viors of carbon materials. The SSA (911.92 m2 g−1) and pore volume
(0.512 cm3 g−1) of TC1200 are basically at the same level with TC
(936.30 m2 g−1, 0.547 cm3 g−1), indicating that the carbonization at
1200 °C has little influence on the pore structure. In addition, the SSA of
commercial AC is 1090 m2 g−1, a little higher than that of TC1200. The
N2 adsorption-desorption isotherms of type I (Fig. 2a) illustrating that
both TC and TC1200 are micropore carbon materials with little
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Applied Surface Science 487 (2019) 189–197
spectra of AC, TC (Fig. S2) and TC1200 (Fig. 2c) are deconvoluted into
five peaks. The D1 band at ≈1340 cm−1 is one of the major peaks to
evaluate the amount of disordered graphene lattices in the graphene
layer edges (A1g symmetry). The D2 (≈1600 cm−1), D3 (≈1531 cm−1)
and D4 (≈1190 cm−1) defect bands represent the in-plane defects (E2g
symmetry), outside-plane defects (amorphous carbon) and the poorly
organized carbon atoms (A1g symmetry), respectively [27–28]. Another
major peak is the G band at ≈1580 cm−1, which represents the degree
of graphitization. The ID/IG value of commercial AC (Fig. 2d) is the
highest among the three materials, evidencing the abundant defects in
AC. The highest graphitization degree of TC1200 is illustrated by the
lowest value of ID/IG (D1/G: 5.95) compared to that of AC (D1/G: 8.68)
and TC (D1/G: 6.49). The high electrical conductivity is crucial for the
superior capacitive behavior. The electrical conductivity of TC1200 is
60.7 S m−1, much higher than that of TC (18.1 S m−1), positively cor-
related with the graphitization degree. The N, O elements distribute
homogeneously on the surface of TC1200, revealed by the EDS ele-
mental mapping picture (Fig. S3). The C]C bonds (284.4 eV) and
quaternary N (401.0 eV) are the dominate existent form of C (95.16%
atomic) (Fig. 2f) and N (0.42% atomic) (Fig. 2g) elements in TC1200,
determined by X-ray photoelectron spectroscopy (XPS) (Fig. 2e). The N
atoms are attributed to the enrichment of N-containing compounds in
the tea leaves without any extra nitrogen sources to be introduced.
Symmetric supercapacitors are fabricated using 6 M KOH aqueous
solution as electrolyte to evaluate the capacitive behaviors of the ma-
terials. The CV curves of TC1200 are much normative than the fusiform
curves of AC and deviated curves of TC within the scan rate of
10–100 mV (Fig. 3a and b). The CV curves of TC1200 present quasi-
rectangular shape with the scan rate increases from 10 mV to 200 mV
(Fig. 3c and d), revealing the fairly ideal storage behavior of double
layer capacitor. The galvanostatic charge-discharge (GCD) profiles of
TC1200 maintain typical symmetric triangle shape with the current
density varies from 4 A g−1 to 30 A g−1 (Fig. 4a), indicating the
X. Song, et al. Applied Surface Science 487 (2019) 189–197

Fig. 4. Galvanostatic charge-discharge profiles of TC1200 (a) and the IR drop of TC and TC1200 (b) under different current densities; (c) capacitance of AC, TC and
TC1200 under different current densities; (d) cycle performance of TC and TC1200 at 4 A g−1 and the galvanostatic charge-discharge profiles at the different cycle
stages (inset).

Table 1 1 A g−1), whereas the reversible capacitance retentions obtained at

Comparison of the cycle performance of previous works with this work. different current densities for TC1200 (81.42% at 30 A g−1) are much
Materials Current Electrolyte Cycle Capacitance
higher than that of TC (64.06% at 30 A g−1) and AC (23.76% at
density number retention 30 A g−1) (Fig. 4c). A capacitance retention of 96.66% is still delivered
(A g−1) (%) for TC1200 after consecutive 16,000 cycles at a current density of
4 A g−1, obviously higher than that of TC (93.41% at 10,000 cycles),
PNHCS [29] 1 6 M KOH 5000 91
benefitted from the superior electric conductivity, and the GCD profiles
NDC [30] 1 1 M LiTFSI 5000 75
NPCHSs [31] 5 6 M KOH 5000 89.1 of TC1200 at different cycle stages are given in the inset of Fig. 4d.
PB-HTC [32] 2 3 M KOH 10,000 89.3 The capacitive performance of TC1200 is quite remarkable com-
HCNs [33] 0.5 6 M KOH 5000 88 pared with various types of carbon-based symmetric supercapacitors
GCDs [34] 10 1 M H2SO4 10,000 90
such as porous nitrogen-doped hollow carbon spheres (PNHCS) [29],
CN-BC [35] 2 6 M KOH 5000 97
NHPC [36] 20 1 M TEABF4 4500 95 nitrogen doped activated carbon from pea skin (NDC) [30], nitrogen
NHPC [36] 10 EMIMBF4 3000 82.8 and phosphorus co-doped carbon hollow spheres (NPCHSs) [31],
CHCPB [37] 2 6 M KOH 3000 91.2 peanut bran derived hierarchical porous carbon (PB-HTC) [32], re-
PCS [38] 4 3 M KOH 5000 94.5 duced graphene oxide (RGO)/MnOx@carbon hollow nanospheres
This work 4 6 M KOH 16,000 96.66
(HCNs) [33], graphene quantum dots (GQDs) [34], bacterial-cellulose-
derived interconnected meso-microporous carbon nanofiber networks
excellent electrochemical reversibility. The GCD profiles of AC and TC (CN-BC) [35], biomass-derived N-doped porous carbon (NHPC) [36],
are presented in Fig. S4 for comparison. The internal resistance (IR) porous carbon from polymer (CHCPB) [37], porous carbon spheres
drop during the discharge curve is related to the resistance and the derived from lignin (PCS) [38] (Table 1). The superior long cycle per-
electroconductivity of the material. The IR drop of TC1200 is much formance for TC1200 is attributed to not only the abundant pore
smaller than that of TC (Fig. 4b), indicating the enhanced electro- structures, but also to the improved conductivity which is proved by the
conductivity and the reversible supercapacitor property. As contrast, electrochemical impedance spectra (EIS) (Fig. S5). The charge transfer
the IR drop of AC is extremely obvious even at low current density of resistance of TC1200 is much smaller than that of TC and AC, reflecting
1 A g−1, demonstrating its poor electric conductivity. The capacitances the lowest equivalent series resistance in the symmetric supercapacitor.
for TC and TC1200 are almost equivalent at 167 F g−1 (current density Moreover, the Nyquist plot of TC1200 in the low-frequency region is
nearly vertical (the phase angle is 88° as demonstrated in Fig. S5b),

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X. Song, et al.
Fig. 5. The contact angle of AC and TC1200.
indicating the quite low ion diffusive resistivity and almost ideal ca-
pacitive behavior of the material [26]. The characteristic time constant
τ0 which reflects the charge-discharge rate of the electrode can be ob-
tained from the operating frequency f0, by the formula τ0 = 1/f0 [39].
The τ0 of TC1200 (2.61 s) is considerably smaller than that of TC
(4.17 s), AC (14.28 s) and several other devices (10–100 s) [40–42]. The
rapid frequency response of TC1200 contributes greatly to its excep-
tional cyclability.
The excellent capacitance performance of TC1200 are ascribed to
not only the higher electric conductivity, but also to the wettability
contributed by the existence of N elements that originated from the tea
leaves [43–44]. The water contact angel of AC and TC1200 are tested to
illustrate the difference in the hydrophilic properties. As presented in
Fig. 5, the contact angel of TC1200 at the initial stage is 29.54°, much
smaller than that of commercial AC (96.26°), and the water droplet
penetrates into the carbon bulk of TC1200 rapidly in a second. Com-
pared with AC, the better wettability of TC1200 is attributed to the
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Applied Surface Science 487 (2019) 189–197
hydrophilic nitrogen functional groups in the bulk phase of the carbon.
The superior wettability and the porosity of the material synergistically
facilitate the electrolyte ion not only diffusion on the surface layer but
also penetrate into the inner layer [24], promoting the double-layer
storage behavior of TC1200.
To evaluate the real performance of TC1200 for general-purpose
under high power conditions, two-electrode symmetric supercapacitor
was assembled in 1 M Na2SO4 electrolyte using TC1200 as both elec-
trodes. All the CV curves of TC1200 exhibit quasi-rectangular shape
without severe distortion as the scan rate increases from 10 mV to
200 mV (Fig. 6a), and the GCD curves are all symmetric triangular
shaped with fairly linear slope (Fig. 6b) at 1–30 A g−1, indicating a fast
and reversible process at the electrode surface in Na2SO4. No obvious IR
drop is observed at each beginning of the discharge curve (Fig. 6b),
apparently demonstrating a quite low internal resistance for TC1200 in
the electrolyte [45]. The capacitance of TC1200 in Na2SO4 is
138 F g−1at 1 A g−1, lower than the value in KOH (167 F g−1),
X. Song, et al.
Fig. 6. (a) CV curves of TC1200 under different scan rate in 1 M Na2SO4; (b) galvanostatic charge-discharge profiles and capacitance under different current
densities; (c and d) comparison of energy and power densities in KOH and Na2SO4 and Ragone plots.
however, the power density and energy density in Na2SO4 are much
higher than that in KOH due to the broader working voltage range. The
power density reaches 23,000 W kg−1 at the energy density of
11 Wh kg−1, and the maximum energy density is 33,500 Wh kg−1 at
20 W kg−1 (Fig. 6c), which are at comparatively high levels among the
carbon materials reported, such as NPCHS [31], biomass-based carbon
[46], graphene quantum dots [34], cellulose-derived meso-microporous
carbon [35], lignin-derived porous carbon spheres [38], biomass-based
3D carbon [47], N-doped hierarchical porous carbon [48] (Fig. 6d). The
excellent electrochemical performance should be ascribed to the por-
osity, high electric conductivity and the excellent wettability of the
material, which synergistically facilitate the double-layer super-
capacitor performance.
4. Conclusions
The construction of a micropore-distributed activated carbon
(TC1200) with high graphitization degree was realized by activation
and carbonization of tea waste. The well-developed porous structure
and the super hydrophilic property synergistically lead to facile elec-
trolyte diffusion, enhancing the double-layer capacitive behavior of the
supercapacitor. The superior electrochemical conductivity prolonged
the cyclability of the electrodes. Symmetric supercapacitor fabricated
from TC1200 delivers an outstanding cycle performance (96.66% ca-
pacitance retention after 16,000 cycles in 6 M KOH), exhibits a max-
imum energy density of 47.86 Wh kg−1 (for a power density of
1580.72 W kg−1) and a maximum power density of 33,494.70 W kg−1
(for an energy density of 19.45 Wh kg−1) in 1 M Na2SO4 electrolyte.
This work provides an easy, affordable, sustainable and accessible
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Applied Surface Science 487 (2019) 189–197
method to produce activated carbons that meet the requirements of the
highly-demanded energy storage devices.
Acknowledgements
This work was supported by Joint Open Fund of Jiangsu
Collaborative Innovation Center for Ecological Building Material and
Environmental Protection Equipment and Key Laboratory for Advanced
Technology in Environmental Protection of Jiangsu Province (No.
JH201812), the National Natural Science Foundation of China (No.
21706283 and No. 21774107), Beijing Talents Foundation (No.
2017000020124G010), Natural Science Foundation of Jiangsu
Province (No. BK20171273), and “Six Talent Peak” High-level Talent
Project (JNHB-068).
Conflict of interest
The authors declare no conflict of interest.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://
doi.org/10.1016/j.apsusc.2019.04.277.
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