Fuel 311 (2022) 122552

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Fuel
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Hierarchical porous carbon derived from coal and biomass for high
performance supercapacitors
Xiaoyun Zhang a, b, 1, Bingkang Sun b, 1, Xing Fan a, d, *, Peng Liang a, Guoming Zhao a,
Binoy K. Saikia c, Xianyong Wei b
a
College of Chemical and Biological Engineering, Shandong University of Science and Technology, Qingdao, Shandong 266590, China
b
Key Laboratory of Coal Processing and Efficient Utilization, Ministry of Education, China University of Mining & Technology, Xuzhou, Jiangsu 221116, China
c
Coal & Energy Group, Materials Science and Technology Division, CSIR-North East Institute of Science and Technology, Jorhat 785006, Assam, India
d
Key Laboratory of Coal Clean Conversion & Chemical Engineering Process of Xinjiang Uygur Autonomous Region, Xinjiang University, Urumqi, Xinjiang 830046, China

A R T I C L E I N F O A B S T R A C T

Keywords: In this work, soluble portions obtained from the co-thermal dissolution (CTD) of rice husk (RH) and coal were
Hierarchical porous carbon used as the carbon precursor for the synthesis of 3D hierarchical porous carbons (HPCs). The electrochemical
Carbon precursors properties of HPCs were tested in supercapacitors as working electrode. HPC-RH3/1 showed a specific capaci­
Mass spectrometry
tance of 352 F/g at 1 A/g and a retention rate of 100% after 10,000 cycles. The composition of the carbon
Electrochemical properties
Supercapacitor
precursors is a key factor determining the characteristics of carbon-based materials. The detailed composition of
carbon precursors was obtained by gas chromatography/mass spectrometry (GC/MS) and Orbitrap MS. The N-
containing organic matters in carbon precursors can improve conductivity and the O-containing compounds can
contribute to pseudocapacitance. According to the MS analysis, the high content of compounds with unsaturated
structures was of benefit to excellent electrochemical properties. The study on the relationships between mo­
lecular compositions of carbon precursors and electrochemical characteristics can give a direction of selection
and optimization of carbon precursors, which further improve the electrochemical performance of carbon
materials.

1. Introduction
Supercapacitors (SCs) have drawn growing attention for their fast
charge/discharge processes, great capability, long cycle life and envi­
ronmentally friendly features [1]. Carbon materials with high chemical
stability, high conductivity, and high specific surface area (SSA), is
considered as a candidate superior electrode material for super­
capacitors [2,3]. Various carbon materials, including active carbon [4],
carbon fiber [5], carbon nanotube [6], graphene and porous carbon [7]
have been widely applied as electrode materials. Among them, hierar­
chical porous carbons (HPCs) with multiscale pores can significantly
improve the capacitance and energy density of supercapacitors [8].
Micro and meso pores facilitate ions transfer, while meso and macro
pores provide mass diffusion pathways [9]. In addition, doping of het­
eroatoms like O and N into carbon materials has been widely used to
improve the electrochemical performance of SCs [10]. Doped N can be
divided into three types, pyrrolic-N, pyridine-N and graphitic-N,
according to the functional groups [11]. Pyrrolic-N and pyridine-N can
act as active sites for electron donors and induce extra pseudocapaci­
tance. Graphitic-N can promote electron transfer and improve conduc­
tivity [12]. O-containing groups, including quinone group (C = O),
phenol group (–OH), ether group (-O-) and carboxylic group (–COOH),
can induce extra pseudocapacitance [13].
Carbon materials synthesized by different precursors exhibit various
morphology structures and electrochemical properties [14–16]. Atha­
nasiou et al. [17] represented a study on the laser-assisted trans­
formation of Corinthian raisins to graphene-like material. Liang et al.
[18] prepared the sulfur and nitrogen co-doped carbon materials
derived from foxtail grass seeds. The obtained carbon material had a
suitable SSA (819 m2/g) and an interconnected porous structure with a
high gravimetric capacitance (358F/g). Coal contains a macromolecular
structure formed by polymerized aromatic rings, and biomass is a nat­
ural product containing abundant heteroatoms. Co-thermal dissolution
(CTD) of coal and biomass is an appropriate strategy to obtain soluble

* Corresponding author at: College of Chemical and Biological Engineering, Shandong University of Science and Technology, Qingdao, Shandong 266590, China.
E-mail address: fanxing@sdust.edu.cn (X. Fan).
1
These authors contribute equally to this work.

https://doi.org/10.1016/j.fuel.2021.122552
Received 25 June 2021; Received in revised form 29 September 2021; Accepted 7 November 2021
Available online 18 November 2021
0016-2361/© 2021 Elsevier Ltd. All rights reserved.
X. Zhang et al.
Fig. 1. (a) Schematic illustration for the synthesis process of HPC-RHX. (b) SEM and (c) TEM images of HPC-RH3/1, (d) high-resolution TEM, and (e-g) elemental
mapping images of HPC-RH3/1.
organic matter, and the synergic effect between coal and biomass in a
CTD process has been probed in Shui’s work [19]. The pyrolysis of
biomass can produce free radicals, which can attack the macromolecular
structure of coal and promote depolymerization.
Mass spectrometry (MS) is an essential method applied in analyzing
complex mixtures like coal and biomass because of the identification of
thousands of unknown compounds at the molecular level [20]. Gas
chromatography/MS (GC/MS) has been applied in revealing composi­
tional information of small molecules with low polarity in complex
mixtures [21]. Orbitrap-MS, a high-resolution MS, can get accurate
molecular information for compounds with medium to high polarities
[22]. The molecular composition of carbon precursors revealed by MS
showed great impact on morphological characteristics and electro­
chemical performances of the carbon-based materials [23]. However,
there are few researches investigating the molecular information of
organic matters in carbon precursors. Thus, the application of MS in the
optimization of precursors is meaningful for the improvement of elec­
trochemical properties for carbon materials.
2
Fuel 311 (2022) 122552
Herein, soluble portions (SPs) obtained from CTD of the mixture of
biomass and coal were used as carbon precursors of carbon materials.
HPCs with well-balanced micro-meso pore structures improved the ca­
pacity and rate performance of supercapacitors. GC/MS and Orbitrap-
MS were applied to analyze the molecular composition of carbon pre­
cursors. MS was used as a bridge connecting the molecular composition
to the electrochemical properties of carbon materials.
2. Experimental
2.1. Material preparation
As shown in Fig. 1a, hierarchical porous carbon derived from rice
husk (HPC-RHX) were prepared from SPs obtained through CTD of rice
husk (RH) and coal. RH and coal mixed with different mass ratios X (X
represent the mass ratios of RH to coal, X = 0/1, 1/3, 1/1, 3/1, 1/0)
were CTD at 300 ◦ C for 2 h and the obtained SPs were named as SP-RHX.
SP-RHX (1.0 g) was mixed with KOH and nano-ZnO (SP-RHX: KOH: ZnO
X. Zhang et al.
Fig. 2. (a) XRD patterns and (b) Raman spectra of HPC-RHX.
= 1:3:3, in wt.%). The mixture was placed in a tubular furnace with a
5 ◦ C/min ramp rate in N2 gas flow. The sample was firstly heated at
300 ◦ C for 30 min. Then, the samples were calcined at 700 ◦ C for 2 h. The
mass ratios of SPs, ZnO and KOH were optimized and the effect of
temperature (500, 600, 700 and 800 ◦ C) on electrochemical properties
were also studied. The detailed preparation process was listed in Sup­
porting Information. The collected products were washed with deion­
ized water. Finally, it was dried at 80 ◦ C for 24 h to obtain HPC-RHX.
2.2. Mass spectrometry
GC/MS (7890/5975, Agilent, Santa Clara, USA) and Orbitrap MS (Q-
Exactive, Thermal-Fisher Scientific, Waltham, USA) were used to
analyze the molecular composition of SP-RHX. The detailed operation
parameters are available in Supporting Information.
2.3. Material characterization
HPC-RHX were measured by X-ray diffraction (XRD), scanning
electron microscopy (SEM), transmission electron microscopy (TEM),
Raman spectroscopy, N2 adsorption–desorption, and X-ray photoelec­
tron spectroscopy (XPS). The detailed operating information of in­
struments are shown in Supporting Information.
2.4. Electrochemical measurement
HPC-RHX, carbon black and polytetrafluoroethylene (PTEF) binder
(8:1:1, wt.%) were mixed in ethanol to form a slurry and coated on
Fig. 3. (a) N2 adsorption/desorption isotherms and (b) pore size distributions of HPC-RHX.
3
Fuel 311 (2022) 122552
nickel foam (1 cm × 1 cm) sheet. After drying, the loaded weight of HPC-
RHX is approximate 1.0 mg. Cyclic voltammetry (CV), galvanostatic
charge/discharge (GCD), electrochemical impedance spectroscopy
(EIS), and cycling stability were measured using a CHI760E electro­
chemical workstation (Chenhua Instrument Co. Ltd., China) and a CT-
4000 battery tester (Neware Electronic Co. Ltd., China). A three-
electrode system was carried out with Pt, HPC-RHX and Hg/HgO as
counter, working and reference electrodes, respectively. The symmetric
supercapacitors consist of two equal carbon electrodes with a piece of
polypropylene membrane. The electrolyte was a 6.0 M KOH aqueous
solution. The calculation formulas of energy storage properties are dis­
played in Supporting Information.
3. Results and discussion
3.1. Materials characteristics
The morphology of HPCs and HPC-RHX was investigated by both
SEM and TEM. As shown in Fig. S1, all HPCs exhibit a porous structure.
The pore morphology of HPC-NZ is mainly micropores, which is ascribed
to the etching effect of KOH. The pore structure in HPC-NK is mainly
mesoporous because the particle size of ZnO template is around 30 nm.
The pore structure of HPC-700-3-3-2 consists of connected hierarchical
porous structures, indicating that KOH and ZnO play different roles in
pore forming process. The etching effect of KOH produces a large
number of micropores and ZnO as a template agent can produce meso­
pores corresponding to its particle size. Fig. 1b-d exhibit an inter­
connected hierarchical porous structure of HPC-RH3/1. The elemental
X. Zhang et al.
Fig. 4. (a) Survey spectrum, (b) high-resolution C1s XPS spectrum, (c) high-resolution N1s XPS spectrum and (d) high-resolution O1s of HPC-RH3/1.
mapping images of a random selected region of HPC-RH3/1 are shown in
Fig. 1e-g, which demonstrate the uniform distribution of C, O and N
elements. The detailed atomic proportions of HPC-RH3/1 can be visu­
alized from Fig. S2. The low N element content is ascribed to the low N
content in SP-RH3/1, which is consist with the ultimate analysis of SP-
RH3/1 (Table S1).
Displayed in Figs. 2 and S3 are XRD patterns and Raman spectra. The
XRD patterns of HPCs and HPC-RHX show the broad (0 0 2) and (1 0 0)
peaks at 2θ = 26◦ and 42◦ , respectively, indicating the existence of
amorphous structures [24]. The Raman spectra display a typical D-band,
G-band and 2D-band peaks of carbon materials (Fig. 2b and Fig. S3b).
The D-band (1345 cm− 1) is related to the disordered carbon textures and
defective graphitic structures, while the G-band (1580 cm− 1) matches to
the graphitic structures [25]. The 2D-band at 2680 cm− 1 is ascribed to
the multi-layer graphene [26,27]. The ratio intensity of D to G bands
(ID/IG) can assess the graphitization degree [28]. The ID/IG values are
around 0.50 (calculated as the integrated area ratio of peak D to peak G),
suggesting a certain degree of graphitization for all samples.
The pore structure and size distribution of HPC-RHX obtained by BET
are shown in Fig. 3a. HPC-RHX exhibit a type Ⅳ isotherm and a hys­
teresis loop, indicating the micro-meso pore structures in HPC-RHX. The
detailed textural parameters are summarized in Table S2. The pore size
distributions in Fig. 3b confirm the co-existence of micropores and
mesopores. Micropores act as the ion-adsorption active sites and meso­
pores work as the channels for ion transport [29]. Shown in Fig. S4 are
the pore structure and size distribution of both HPC-NK and HPC-NZ.
HPC-NZ exhibits a type I isotherm, indicating that the pore
morphology of HPC-NZ is mainly micropores. For HPC-NK, micropores
account for the main pore structure, which is consist with the results of
SEM and TEM.
XPS was applied to analyze the elemental composition on the surface
of HPC-RH3/1 and HPC-700-3-3-2, which are shown in Fig. 4 and S5,
4
Fuel 311 (2022) 122552
respectively. The XPS surveys of HPC-RH3/1 disclose the presence of C, O
and N elements, while the XPS surveys of HPC-700-3-3-2 only presents
two peaks at 284.9 and 532.4 eV, referring to the peaks of C1s and O1s,
respectively [30]. The XPS data of HPC-RH3/1 are listed in Table S3. The
deconvoluted C1s spectrum of HPC-RH3/1 (Fig. 4b) consists of four peaks
with a dominant peak centered at 284.4 eV and assigned to C = C bond.
The other three peaks at the binding energy of 285.0, 285.9 and 289.4
eV are ascribed to C–C, C-O and C-N bands [31]. In Fig. 4c, the O1s
spectrum can be divided into four distinct peaks at 531.4 eV, 532.3 eV,
533.2 eV, and 536.9 eV, corresponding to C = O, O–H, C-O and H2O
bands [32]. The high-resolution XPS spectrum of N1s can be deconvo­
luted into a main peak of pyrrolic-N (400.1 eV) and two minor peaks of
pyridinic-N (398.5 eV) and graphitic-N (401.2 eV) [33,34]. Compared
with HPC-700-3-3-2, the O and N element contents of HPC-RH3/1 are
higher and benefit to the improvement of electrolyte surface tension and
electrode surface wettability [35,36].
3.2. Electrochemical characterization
The electrochemical performances of HPCs and HPC-RHX were
measured in a three-electrode system. Fig. S6 lists the CV curves, GCD
curves and Nyquist plots of HPCs prepared under different conditions.
HPC-700-3-3-2 shows the best electrochemical performance among
them. With the enhancement of temperature, the capacitance value in­
creases and reaches the maximum at 700 ℃. A high carbonization
temperature will cause the collapse of pores in carbon material, resulting
in the decrease of specific surface area. KOH and ZnO mainly affect the
morphology and pore structure. HPC-700-3-3-2 has the highest value of
Smicro/Smeso, indicating a well-balanced micro-meso pore structure
(Table S2) [37]. Fig. 5a shows the CV curves of HPC-RHX, which exhibit
a quasi-rectangle shape, indicating electric double layer capacitance
(EDLC) behaviors. The weak and broad peaks in CV curves correspond to
X. Zhang et al. Fuel 311 (2022) 122552

Fig. 5. Electrochemical characteristics of a three-electrode system of HPC-RHX. (a) CV curves at 10 mV s− 1, (b) GCD curves at 1A g− 1, (c) Nyquist plots, (d) CV curves
at different scan rates for HPC-RH3/1, (e) GCD curves at different current densities for HPC-RH3/1, (f) specific capacitance at different current densities.

pseudocapacitance behaviors resulting from the O-containing functional
groups in HPC-RHX [38,39]. As shown in Fig. 5b, the superior capaci­
tance of HPC-RHX was further measured by GCD. All the curves show
symmetric linear shapes, indicating a good capacitive performance.
HPC-RH3/1 electrode obtains a high capacitance of 352 F/g. Nyquist
plots in Fig. 5c are composed of a semicircle (high frequencies) and a
straight line (low frequencies). A lower solution resistance (Rs) value
and a steeper linear slope of HPC-RHX mean a lower resistance and a
faster ion transfer, respectively. In Fig. 5d, CV curves of HPC-RH3/1
maintain a quasi-rectangle shape even at 200 mV/s, which is profited
from its good capacity. The shape of GCD curves retains symmetrical
triangle at 20 A/g, which reveals an excellent capacitive behavior and
electrochemical reversibility (Fig. 5e). As shown in Fig. 5f, HPC-RH3/1
obtains a capacitance of 268 F/g at 20 A/g.
Furthermore, a two-electrode symmetric supercapacitor device were
also fabricated. The CV curves and GCD curves maintain the original
shape under a high scan rate and a high current density (Fig. 6a and 6b).
As presented in Fig. 6c, after 10,000 cycles, the stability of HPC-RH3/1
remains 100%. After the cycle stability test, the morphology of HPC
basically remain unchanged and the uniform distribution of C, O and N
elements in HPC-RH3/1 is displayed in Fig. S7. In addition, from the
Ragone plot (Fig. 6d), the energy density reached 6.98 Wh/kg at a power
density of 500 W/kg.
3.3. Molecular characteristics
The organic matters in carbon precursors can determine the
morphological characteristics and electrochemical properties of pre­
pared carbon materials. In Fig. S8, the yields of SP-RHX increase with the
mass ratio of RH to coal. Therefore, small molecules in biomass are

5
X. Zhang et al.
Fig. 6. Electrochemical characteristics of a two-electrode system of HPC-RH3/1. (a) CV curves at different scan rates. (b) GCD curves at different current densities. (c)
Cycling stability performance at a current density of 10 A g− 1. (d) Ragone plot.
Fig. 7. Relative abundance distribution of all classes in SP-RHX obtained by
GC/MS.
easier to be dissolved under the same condition compared to coal. The
relative abundance distribution of all classes in SP-RHX obtained by GC/
MS is displayed in Fig. 7. The bars in black color represent O-containing
compounds, which can be divided into five types, including alcohols,
ketones, phenols, esters and aldehydes. In Fig. 7, esters show the highest
content in SP-RHX. SP-RH3/1 exhibits the highest amount of N- and O-
containing compounds among all SPs, leading to the high content of O
and N elements in HPC-RH3/1. O and N heteroatoms doping into the
carbon backbone is an effective strategy to increase the capacitive per­
formance. The N content in SP-RH3/1 is the highest among all samples
and HPC-RH3/1 shows the best capacitive performance. N-containing
6
Fuel 311 (2022) 122552
species exist in three forms, pyrrolic-N, pyridine-N and graphitic-N.
Pyrrolic-N and pyridine-N can act as active sites for electron donors
and induce extra pseudocapacitance. Graphitic-N can promote electron
transfer and improve conductivity. O-containing groups, including
quinone group (C = O), phenol group (–OH), ether group (-O-) and
carboxylic group (–COOH), can induce extra pseudocapacitance through
the following chemical reactions [40]:
− C − OH ↔ − C = O + H+ + e−
− COOH ↔ − COO + H+ + e−
− C = O + e− ↔ − C − O−
Figs. 8, S9 and S10 display double bond equivalence (DBE) plots
obtained from Orbitrap MS spectra. The color mapping, from red to blue,
represents the relative abundance of organic compounds in SPs. DBE
value is an indicator of the degree of unsaturation in SP-RHX. In Fig. 8c,
the compounds mainly concentrate in the red rectangle area (4 ≤ C ≤
20), demonstrating a high content of unsaturated structures in SP-RH3/1.
The DBE plots derived from the mass spectra of ON-, O- and N-con­
taining compounds are shown in Fig. S9 and S10. With the enhancement
of mass ratio of RH to coal, the content of N-containing compounds in
SP-RHX increases and reaches the highest value in SP-RH3/1.
4. Conclusions
HPCs were prepared from soluble portions obtained through a co-
thermal dissolution process of coal and rice husk. The carbonization
temperature, carbonization time, and the mass ratio of SP, ZnO and KOH
for material preparation were optimized. Among HPCs, HPC-RH3/1
showed a high specific capacitance and a great retention rate. Mass
spectrometry was applied to build relationships between the molecular
X. Zhang et al.
Fig. 8. DBE plots of SP-RHX. (a) SP-RH1/3, (b) SP-RH1/1, (c) SP-RH3/1 and (d) SP-RH1/0.
composition of carbon precursors and the electrochemical property of
carbon-based materials. The N-containing compounds in carbon pre­
cursors improved conductivity, and the O-containing compounds
contributed to pseudocapacitance and increased wettability. A high
content of unsaturated structure was of benefit to the perfect electro­
chemical properties. The elucidation of relationships between molecular
composition of precursors and electrochemical performance of carbon
materials will give direction in carbon precursor optimization to prepare
supercapacitors with excellent performance.
CRediT authorship contribution statement
Xiaoyun Zhang: Conceptualization, Methodology, Writing – orig­
inal draft. Binkang Sun: Conceptualization, Methodology, Writing –
original draft. Xing Fan: Conceptualization, Writing – review & editing,
Supervision. Peng Liang: Software, Validation. Guoming Zhao: Data
curation. Binoy K. Saikia: Writing – review & editing. Xianyong Wei:
Supervision.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgements
This work was supported by the National Natural Science Foundation
of China (Grant 21676293), the Natural Science Foundation of Shan­
dong Province (Grant ZR202103070181), and the Key Project of Joint
Fund from National Natural Science Foundation of China and the Gov­
ernment of Xinjiang Uygur Autonomous Region (Grant U1503293).
7
Fuel 311 (2022) 122552
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.fuel.2021.122552.
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