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Article history: A simple, effective, and scalable mix and pyrolysis process was developed for preparing rice husk-derived
Received 4 July 2017 porous carbon. The process involves only mixing and pyrolyzing of carbon–silica composites (product of
Revised 20 September 2017
pre-carbonized rice husk) and Polytetrafluoroethylene (PTFE) powders under inert atmosphere to form
Accepted 1 October 2017
porous carbon materials without any SiO2 residue. The fabrication process does not use any toxic or cor-
Available online xxx
rosive solution to etch the SiO2 , which was more suitable for large scale production. The obtained porous
Keywords: carbon was endowed a desirable specific surface area (1550 m2 /g) and porous structure with high meso-
Rice husk porosity of 52%. Electrochemical investigation measurements showed that the obtained porous carbon
Carbon materials represents a good electrode candidate for supercapacitor, which displayed a high specific capacitance of
Electrode 220 F/g at a current density of 0.5 A/g. In addition, the electrode displayed excellent cycling stability with
SiO2 a capacitance retention of about 98% over 10,0 0 0 cycles.
Supercapacitor
© 2017 Taiwan Institute of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
1. Introduction trode materials for energy storage due to their high specific sur-
face area, high thermal and chemical stability, excellent conductiv-
With the growing ultilize of energy and strengthening of ity and low cost [8–10]. Biomass derived porous carbon materials
people’s environmental protection consciousness, researchers are have been prepared and used in electrochemical energy systems
constantly looking for new technology for developing renewable due to their easy regeneration, abundant and low cost [7,11,12].
energy sources. Except that develop new energy, energy storage Until now, various biomass materials have been used as the car-
technology also should be paid attention to enhance the effec- bon sources to prepare porous carbon, including peanut shell [13],
tive utlization of renewable energies. Supercapacitors also called fungus [14], cotton wool [15], pomelo peel [16,17], shrimp shells
electrochemical capacitors have attracted a great deal of attention [18], and so on.
among various electrical energy storage devices due to their high Rice husk, the hard protecting covering of grain, is considered
power density, fast charging-discharing time and long cycling as the agricultural waste of rice. Unfortunately, most of rice husk
life [1,2]. According to established charge storage mechanisms, is burn out, which would cause the environmental pollution. The
supercapacitors can be classfied into two kinds: electrochemical compositions of rice husk are cellulose(38%), hemicelluloses(18%),
double layer capacitors and pseudocapacitors. The former stores lignin(22%) and SiO2 [19]. Thus, it can be utilized as the carbon
electric energy based on the electrosorption of electrolyte ions at precursor to prepare the activated carbon materials under an inert
the electrodes/electrolyte interfaces, whereas the latter primarily atmosphere. Actually, during the past decade, rice husk has been
originates from fast superficial Faradaic redox reactions between widely studied and prepared into porous carbon materials. How-
the electrode materials and electrolyte ions [3–5]. ever, in order to obtain silica-free rice husk-derived carbon mate-
Carbon materials have attracted great attentions in catalysis, rials, silica are removed using HF or alkaline solution (NaOH, KOH)
adsorption, energy storage and conversion [6,7]. During the past at elevated temperature [19–21]. Unfortunatly, HF is highly toxic
decade, porous carbon materials are widely studied as the elec- and bad for human health, while alkaline solution treatment is
time consuming and strong corrosive. Obviously, HF solution and
∗
alkaline solution are the major obstacle in industrial applications.
Corresponding authors at: Key Laboratory of Optoelectronic Chemical Materials
and Devices, Ministry of Education, Jianghan University, Wuhan 430056, China What’s more, most researches used a large number of activating
E-mail addresses: liangjy2004@126.com (J. Liang), caosome@126.com (Y.-C. Cao). agent to increase the specific surface area of porous carbon, which
https://doi.org/10.1016/j.jtice.2017.10.001
1876-1070/© 2017 Taiwan Institute of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
Please cite this article as: J. Liang et al., In situ SiO2 etching strategy to prepare rice husk-derived porous carbons for supercapacitor
application, Journal of the Taiwan Institute of Chemical Engineers (2017), https://doi.org/10.1016/j.jtice.2017.10.001
JID: JTICE
ARTICLE IN PRESS [m5G;October 23, 2017;14:2]
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(002)
Intensity (a.u.)
report an expeditious strategy to prepare high performance rice
husk-derived porous carbon via Polytetrafluoroethylene (PTFE) in-
(101)
situ silica etching process without using any toxic HF solution or
(101)
alkaline solution. Compared with the traditional rice husk based PRHC
porous carbon material preparation, the present method integrates
the rice husk carbonization and SiO2 etching into one procedure,
which affords a convenient and energy-saving route to the synthe-
(200)
sis of rice husk based porous carbon. The as-obtained carbon ma-
(111)
(102)
terials are tested as the electrode materials for supercapacitor. This
method also provides a paradigm for the SiO2 etching strategy. C-SiO2
JCPDS No. 39-1425
2. Experimental
10 20 30 40 50 60 70 80 90
2.1. Preparation of rice husk-derived carbon (RHC) 2 theta (degree)
The rice husk used in this work was bought from Lvhuai agri- Fig. 1. XRD patterns of C–SiO2 , CRHC and PRHC.
The morphology of the sample was characterized by field The crystal structure of the rice husk after pre-carbonzation
emission scanning electron microscopy (FESEM, Hitachi SU8010) was investigated by XRD. As shown in Fig. 1, the crystalline SiO2
equipped with energy dispersive spectroscopy (EDX) system. X-ray refraction peaks (JCPDS No. 39-1425) can be clearly detected. This
diffraction (XRD) was recored with Rigaku D Max/20 0 0 PC powder suggests that silica–carbon composite is formed during thermal
diffractometer with Cu Kα radiation. Raman spectra were recored carbonization. It is interesting to find that SiO2 refraction peaks are
on the Raman Scattering Spectroscopy (Renishaw 20 0 0 system) us- disappeared after pyrolizing the mixture of carbon–silica sample
ing 632 nm laser light source. The electrical conductivity of the and PTFE powder, while two broad diffraction peaks centered at
sample was measured using a four-point probe meter (Keithley, 25 and 44° are attributed to the characteristic diffraction peaks of
2400). Thermogravimetric analysis (TGA) was performed on a Ther- graphite of the (002) and (101) planes, respectively. Similar to for-
mal Analysis thermogravimetric analyser at a heating rate of 5 and mer studies, XRD result also indicates that SiO2 species can be re-
10 °C/min under nitrogen and air atmosphere, respectively. Nitro- moved thoughly by HF solution treatment. What’s more, compared
gen adsorption–desorption isotherms were conducted at 77 K on with the CRHC, the (002) diffraction peak of PRHC is more broad,
a physical adsorption instrument (Micromeritics, ASAP 2020). The indicating that the crystalline structure is markedly destroyed by
sample was degassed at 150 °C for 10 h before the analysis. PTFE treatment in the chemical etching process. TG analysis was
also performed to test the residual SiO2 . From Fig. S2, it is demon-
2.3. Electrochemical tests strated that the weight dropped to zero after 800 °C, further re-
vealing that SiO2 can be clearly etched through the PTFE treatment
Prior to electrode preparation, commercial nickel foam was pre- during the pyrolysis process.
treated in a 3 M HCl solution with sonication for 10 min to remove The morphology and structure of samples was examined by
the NiO layer, and then washed thoroughly with deionized wa- SEM as shown in Fig. 2. It can be seen from Fig. 2a to c that an
Please cite this article as: J. Liang et al., In situ SiO2 etching strategy to prepare rice husk-derived porous carbons for supercapacitor
application, Journal of the Taiwan Institute of Chemical Engineers (2017), https://doi.org/10.1016/j.jtice.2017.10.001
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Fig. 2. Digital photos of (a) fresh rice husk, (b) carbon–silica composites, and (c) PRHC. (d, e) SEM images of carbon–silica. (f, g) SEM images of CRHC. (h, i) SEM images of
PRHC.
obvious physical change has occurred following the annealing and served in the sample (Fig. 2i); these opened pores may be gen-
etching procedures, going from yellow rice dusk to a black powder. erated from the decomposition gases of PTFE. This porous strc-
Fig. 2d and e demonstrate the corresponding SEM image of the ture also can be served as the ion buffers and shorten the elec-
outside and inside surface of precarbonized sampe (carbon–silica trolyte ions diffusion pathway to the active sites [25,26]. Therefore,
composite), respectively. As can be seen, the nature microstruc- a high specific surface area and a hierarchical porous structure in
ture of rice husk can be well preserved after pre-carbonization. the PRHC are expected. In order to observe the chemical composi-
There are many bulges with globular structure on the outside sur- tion of all the specimens, EDX test was also performed in this pa-
face and the inside surface is relative smooth. As the SEM im- per. As expected, the corresponding EDX spectrum (Fig. S3) shows
ages in Fig. 2f and g illustrate, CRHC broke into many non-uniform that C and O are the major elements in the PRHC, indicating the
particles with wide particle size distribution. For the PRHC, inter- complete removal of the SiO2 , which is also confirmed by TG anal-
estingly, the bulged structure can be retained, but the surface of ysis in Fig. S2.
bulges become more rough and much more pores can be already Raman spectroscopy was employed to evaluated the physical
observed from the SEM micrograph of the PRHC sample (Fig. 2h), structural differences of the samples. As can be seen in Fig. 3,
in constract to the relative smooth surface of pre-carbonized rice all the samples display two distinct Raman peaks at around 1350
husk shown in Fig. 2d. Furthermore, porous structure can be ob- and 1580 cm−1 , which corresponding to the D band and G band,
Please cite this article as: J. Liang et al., In situ SiO2 etching strategy to prepare rice husk-derived porous carbons for supercapacitor
application, Journal of the Taiwan Institute of Chemical Engineers (2017), https://doi.org/10.1016/j.jtice.2017.10.001
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Table 1.
Pore structure parameters of CRHC and PRHC.
Sample Stol (m2 /g) Smicro (m2 /g) Smeso (m2 /g) Ratioa Pore volume Dp (nm)b
(cm3 /g)
a b
Fig. 4. (a) Nitrogen adsorption/desorption isotherms and (b) pore size distribution of CRHC and PRHC.
Please cite this article as: J. Liang et al., In situ SiO2 etching strategy to prepare rice husk-derived porous carbons for supercapacitor
application, Journal of the Taiwan Institute of Chemical Engineers (2017), https://doi.org/10.1016/j.jtice.2017.10.001
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a b
Fig. 5. Cyclic voltammetry curves of (a) CRHC and PRHC at a scan rate of 10 mV/s and (b) PRHC electrode at increasing scan rates.
Please cite this article as: J. Liang et al., In situ SiO2 etching strategy to prepare rice husk-derived porous carbons for supercapacitor
application, Journal of the Taiwan Institute of Chemical Engineers (2017), https://doi.org/10.1016/j.jtice.2017.10.001
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a b
Fig. 7. (a) Galvanostaticcharge–discharge curves of PRHC at various current densities. (b) Specfic capacitances of CRHC and PRHC electrode as functions of various current
densities.
a b
Fig. 8. (a) Cyclic stability of CRHC and PRHC. (b) Galvanostatic charge–discharge curves of PRHC electrode at 1st and 10,0 0 0th cycles.
suggest that the porous structure is suited for the fast ions dif-
fusion of PRHC electrode under high current density. The large
amount of micropores provides abundant surface areas to gener-
ate electric double layers. Furthermore, from the above SEM im-
age observation, there are many macropores in the PRHC. The
opened macroporous structure can lessen the electrolyte ions dif-
fusion pathway to the active sites, and hence benefit for improv-
ing the rate capability [39]. More importantly, from a comprehen-
sive comparison of the PRHC electrode vs. recently published rice
husk-derived porous carbon materials, the PRHC electrode obvi-
ously exhibits comparable and/or even higher specific capacitance
than those listed in Table S1. However, most of them were pre-
pared using activating agent to increase the specific surface area.
It should be strengthen that our prepartion process does not use
any activating agent.
The cycling stability is also a critical parameter for the practical
supercapacitor applications. The cycling stability of RHC electrode
was performed at a current density of 2 A/g. As shown in Fig. 8a,
the specific capacitance of PRHC decreased slowly, and about 98%
of the initial specific capacitance is retained after 10,0 0 0 cycles.
Fig. 9. Nyquist plots of the CRHC anf PRHC electrodes. The inset shows locally en-
This demonstrates that the PRHC has a relatively excellent long- larged Nyquist plosts in the high frequency region.
term stability. Fig. 8b shows the charge–discharge curves of the
first cycle and the 10,0 0 0th cycle. Notably, no obvious change can
be found, further confirming the outstanding cycling stability of Electrochemical impedance spectroscopy (EIS) is an effective
the electrode. method to obtain the kinetic performance information of the elec-
Please cite this article as: J. Liang et al., In situ SiO2 etching strategy to prepare rice husk-derived porous carbons for supercapacitor
application, Journal of the Taiwan Institute of Chemical Engineers (2017), https://doi.org/10.1016/j.jtice.2017.10.001
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trodes. Fig. 9 shows the corresponding Nyquist plots of CRHC and City and Hubei Province Innovative Young Research Team in Uni-
PRHC electrode. Both of plots are composed of a semicircle in the versities (T201318).
high frequency region, relating to the charge transfer resistance
at the interface, and an inclined line in the low frequency region, Supplementary materials
corresponding to the electrolyte ions diffusion resistance [40]. The
smaller the semicircle, the lower is the charge transfer resistance, Supplementary material associated with this article can be
and the steeper the inclined line, the lower is the electrolyte ions found, in the online version, at doi:10.1016/j.jtice.2017.10.001.
diffusion resistance [41]. Compared to the CRHC electrode, the
semicircle of PRHC electrode is smaller and its inclined line is
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application, Journal of the Taiwan Institute of Chemical Engineers (2017), https://doi.org/10.1016/j.jtice.2017.10.001
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Please cite this article as: J. Liang et al., In situ SiO2 etching strategy to prepare rice husk-derived porous carbons for supercapacitor
application, Journal of the Taiwan Institute of Chemical Engineers (2017), https://doi.org/10.1016/j.jtice.2017.10.001