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 Page 1 of 15 New Journal of Chemistry
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Water bamboo-derived porous carbons as electrode materials for

supercapacitors

New Journal of Chemistry Accepted Manuscript

Jiangfeng Li, Qingsheng Wu*

Department of Chemistry, Key Laboratory of Yangtze River Water Environment, Ministry of Education,
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Tongji University, Shanghai 200092, PR China

Abstract:

The microporous carbon materials with specific surface area as high as 2352 m2 g-1 were

synthesized by the carbonization of KOH-pretreated partially carbonized water bamboo at 800 ℃

under N2 atmosphere for supercapacitor application. In particular, the carbon materials synthesized at

2:1 weight ratio of KOH and pre-treated carbon exhibited excellent performance with maximum

specific capacitance of 268 F g-1 at a current density of 1 A g-1 in 6 M KOH electrolyte and retained up

to 222 F g-1 even at a current density of 10 A g-1. In addition, this material also showed good capacity

retention of 97.28 % over 5000 cycles at a current density of 10 A g-1. The excellent electrochemical

properties could be due to high specific surface area, abundant pore volume, proper pore size

distribution and some oxygen groups.

1. Introduction

Nowadays, the problem of energy shortage is getting more and more serious. Supercapacitors as

the new energy storage devices have received amount of attention because of their high power density

(103-104 WKg-1), long cycling life (>106 cycles), high specific capacitance and short charging time 1-4
.

Depending on charge-storage mechanism, supercapacitors can be divided into two classes, i.e.

* Corresponding author. Tel: +86 21 65982620, Fax: +86 21 65981097.

E-mail address: [email protected] (Q. Wu ).

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pseudocapacitors and electrochemical double-layer capacitors (EDLCs) 5. In the pesudocapacitor, the

capacitance comes from a Faradaic process, indicating that the storage is based on reduction-oxidation

New Journal of Chemistry Accepted Manuscript

reaction 6. However, pseudocapacitors suffer from poor electrical conductivity, low power density and

7, 8
lack of stability .The capacitance of EDLCs comes from the adsorption of electrolyte ions at
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electrode and electrolyte interfaces 9. Therefore, specific surface area and pore structure of electrodes

10, 11
are two important factors which influence the energy storage of EDLCs . In recently years,

activated carbon materials, which can be synthesized by template method and chemical/physical

activation, have achieved high EDLCs performances 12-16. The well-defined pore size distribution, high

specific surface area and good crystallinity of activated carbons are keys to exhibiting the

electrochemical capacitance performance of such supercapacitors 2, 17, 18.

Recently, biological materials have been attracting much attention in the fabrication of activated

carbons for energy applications. Compared with the conventional raw materials (such as petroleum

coke, tar pitches and coal), biomasses have three advantages: environmental friendly, low cost and

19-21 22, 23 24 25
renewables . Several biomass materials such as cornstalks , durian shell , cherry stone ,

gelatin 26, coffee bean 27, eucalyptus wood saw dust 28, etc are employed to synthesize activated carbons

with high specific surface area and porosity. For instance, high performance activated carbon derived

from tamarind fruit shell showed a specific capacitance of 412 F g-1 and an energy density of 9.166 Wh

Kg-1 in aqueous 1 M H2SO4 19. Activated carbon materials via high-temperature carbonization of neem

(Azadirachta indica) dead leaves yield a very high specific capacitance of 400 F g-1 and an energy

density of 55 Wh Kg-1 in 1 M H2SO4 29

. Zhou et al. successfully utilized natural loofah sponges as

precursors to fabricate three-dimensional (3D) porous carbon materials 30.

Water bamboo (Zizania Latifolia), a kind of vegetable, is large-scale cultivated along Yangtze
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River and the south areas. Despite of being an inexpensive and abundant precursor for producing

activated carbon, water bamboo has not been explored in any electrochemical application. In this study,

New Journal of Chemistry Accepted Manuscript

we demonstrate the synthesis of activated carbon materials by the carbonization of KOH-pretreated

water bamboo under N2 atmosphere at high temperature. The porous carbon materials activated by
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KOH at high temperature can exhibit larger surface areas, abundant micropores and higher content of

oxygen groups31, 32. The as-prepared water bamboo-derived carbon (WBC) materials possess a high

specific surface area induced by KOH activation.

2. Experimental

2.1 Materials

The water bamboo was purchased from market in Shanghai. Hydrochloric acid, potassium

hydroxide, ethanol, graphite powder were purchased from Shanghai Chemical Reagents Co., Ltd.

Deionized water was used throughout the experiments. Pure nitrogen was bought from Shanghai BOC

Special Gases Sales Service Co., Ltd. Nickel foil was bought from Shanghai Hongxiang Plant.

Polytetrafluoroethylene (PTFE) solution was obtained from Shanghai 3F New Materials Co., Ltd.

2.2 Synthesis of Water bamboo derived porous carbon

Scheme 1 shows the procedure to synthesize the water bamboo derived porous carbon materials.

The peeled water bamboo was washed with deionized water, cut into a small debris, and dried at 60 ℃

in a vacuum oven. The dried debris was preheated at 450 ℃ for 2 h in a quartz tube furnace under

constant N2 flow. The pre-carbonization materials were ground to powder, mixed with KOH in

different proportions, and carbonized in a ceramic crucible from room temperature to 800 ℃ for 2 h

under an nitrogen atmosphere. The carbonized products were immersed in excess 1 M HCl solution,

washed several times with hot deionized water, and finally dried at 80 ℃. The weight ratio of KOH to
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WBC is from 0 to 3 and thus obtained carbons are denoted as WBC-1, WBC-1, WBC-2 and WBC-3,

respectively.

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Scheme 1 Schematic for the fabrication of porous carbon materials from water bamboo.

2.3 Preparation of the electrodes

To prepare the working electrode, the composite (85 wt %), graphite powder (10 wt %) and PTFE

(5 wt %) were mixed homogeneously with deionized water. The mixture was coated onto the nickel

foam substrate (1cm×1cm) at 10 MPa and dried at 80 ℃ in a vacuum oven to remove the deionized

water. The active material mass of the electrode is about 1.2 mg. The electrochemical analysis was

investigated using the three-electrode cell systems, and a Pt foil and Ag/AgCl electrode were used as

the counter and reference electrodes in 6 M KOH electrolyte, respectively.

2.4 Characterization techniques

The prepared materials were investigated by scanning electron microscopy (SEM, Phenom

Pro-G2, Netherlands) and transmission electron microscopy (TEM, JEOL JEM-2100, Japan). Powder

X-ray diffraction (XRD) was got on Bruker Focus D8 diffract-meter with Cu Kα radiation (40 kV,

λ=0.15418 nm) between 10 and 70°. The adsorption amounts were carried out using Micromeritics

Tristar 3000 gas adsorption analyzer. The specific surface area was calculated through a single-point

Brunauer-Emmett-Teller (BET) method and the pore size distributions were obtained by

Barret-Joyner-Halenda (BJH) model from the desorption branch of the isotherms. High temperature

was performed with the samples of 10 mg by TPD (temperature programmed desorption) experiments
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under a temperature of 850 °C keep 0.5 h (heating rate 10 ℃ min-1) with a continuous He flow. The

evolution of CO and CO2 was analyzed by mass spectrometer (MS, Hiden HPR20, England).

New Journal of Chemistry Accepted Manuscript

Electrochemical measurements were tested by a CHI 660E electrochemical workstation (ChenHua

Corp., Shanghai, China).

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3. Results and discussion

3.1 Sample characterization

It is well known that the surface morphology and structure are two important factors influencing

the specific capacitance for carbon-based electrochemical materials. Fig. 1A, B and C display the SEM

images of the obtained samples, respectively. All the samples exhibit highly irregular surface and

abundant porous morphology by activating the pre-carbonized water bamboo with KOH as activator.

As depicted in Fig. 1A, the surface of WBC-1 is rough and lax with large pore size more than 5 um. At

KOH/WBC ratio of 2, WBC-2 shows a loose structure with distribution on the surface with massive

pores (Fig. 1B). But at KOH/WBC ratio of 3, the number of holes distribution on the surface is reduced

seriously, which bring down the specific surface area for ion adsorption and transportation (Fig. 1C).

Therefore, the KOH amount should be properly selected to obtain abundant and interconnected porous

structure which can significantly enhance the ability of fast charge and mass transport at high current

33, 34
density . The microstructure of WBC-2 was investigated by TEM. As shown in Fig. 1D, WBC-2

has abundant porous structure with the pore sizes less than 2 nm, which provides an effective volume

35, 36
for the absorption of electrolyte ions . Fig. 2 shows the powder XRD spectra of these materials.

There are two diffraction peaks clearly observed at 23.6 o (graphitic peak) and 44.5o for all WBC

samples because of the formation of high levels of in-plane condensation, which should greatly

enhance the electrical conductivity 37. On closer examination, the crystallinity of WBC-3 is decreased
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obviously with the broadening of graphitic peak 15.

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Fig. 1 SEM images of WBC-1 (A), WBC-2 (B) and WBC-3 (C); and TEM image of WBC-2 (D).

Fig. 2 XRD patterns of samples WBC-1, WBC-2 and WBC-3.

Fig. 3A shows the microstructural characteristics of WBC-1, WBC-2 and WBC-3, analyzed by

using nitrogen adsorption/desorption isotherms. The shapes of all samples exhibit a type I isotherm,

38, 39
indicating the microporous character of as-prepared samples . Fig. 3B shows the pore size

distributions of the samples. As depicted in Fig. 3B, these samples have similar pore size distributions,

which range from 1.5 to 5 nm. The porous properties of these carbon materials are displayed in Table 1.

It can be observed that the BET specific surface areas of KOH-pretreated carbon materials are larger

than the direct carbonized materials. At high temperature, KOH can react with carbon to generate H2,
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CO and CO2, which has contributed to the formation of pores40. The reaction mechanism is followed：

6KOH + 2C → 2K + 3H 2 + 2K2CO3 （1）

New Journal of Chemistry Accepted Manuscript

K2CO3 → K2O + CO2 （2）

CO2 + C → 2CO （3）

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K2CO3 + 2C → 2K + 3CO （4）

K2O + C → 2K + CO （5）

The measured BET specific surface areas are 1846, 2352 and 1905 m2 g-1 with the pore volumes are

0.95, 1.17 and 0.93 cm3 g-1 for WBC-1, WBC-2 and WBC-3, respectively. It could be seen that WBC-2

had the highest specific surface area with largest micropore volume among all samples. At a higher

KOH/WBC ratio, the surface area and micropore volume were reduced badly because of the collapse

40
of small pore walls during the KOH activation process . The samples could obtain an excellent

electrochemical performance due to the coexistence of micropores and mescropores. The large specific

surface area and high micropore volume of WBC-2 contributes to the transfer and storage of electrolyte

ion.

Fig. 3 (A) Nitrogen adsorption/desorption isotherms and (B) pore-size distribution of WBC-1, WBC-2

and WBC-3.

Table 1 Specific surface area and pore characteristics of the obtained samples.

Samples SBET Slangmuir Vpore VMicro Daver

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[m2 g-1] [m2 g-1] [cm3 g-1] [cm3 g-1] [nm]

WBC-0 683 926 0.4 0.31 2.3
WBC-1 1846 2539 0.95 0.88 1.93
WBC-2 2352 3308 1.17 1.11 1.99

New Journal of Chemistry Accepted Manuscript

WBC-3 1905 2639 0.93 0.89 1.84
SBET: BET surface area.
Slangmuir: Langmuir surface area.
Vpore: Total pore volume.
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VMicro: Micropore volume (below 2 nm pore size).

Daver: Average pore size.
3.2 Electrochemical properties

The electrochemical performance of these WBCs was characterized by cyclic voltammetry (CV)

analysis in 6 M KOH electrolyte in the range of -0.8 to -0.1 at different scan rates (Fig. 4). As depicted

in Fig. 4, all CV curves show almost a rectangular shape at the scan rate of 50 mV s-1. When at the scan

rate of 100 mV s-1, the CV curves of these samples are a departure from rectangular shape on account

41
of large ohmic resistances . Compared with the CV curves of WBC-1 and WBC-3, the rectangular

shape of WBC-2 is a less distorted due to its high surface area and abundant micropores that promoted

ion diffusion into inner pores. Among the studied results, the pore structure of WBC-2 is more suitable

for ions of electrolytes transfer and adsorption than other two samples, which indicates that WBC-2

was the promising electrode materials for supercapacitors.

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New Journal of Chemistry Accepted Manuscript

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Fig. 4 Cyclic voltammetry curves of WBC-1, WBC-2 and WBC-3 at different scan rates.

Galvanostatic charge and discharge technique is an effective method to investigate the

performance of these samples-based electrode materials. Fig. 5 shows the galvanostatic charge and

discharge curves and specific capacitances of WBC-1, WBC-2 and WBC-3 at different current

densities. For quantitative considerations, the specific capacitance is calculated using the following

equation:

I × △t
Cs = ( Fg −1 )
△V × m

Where I is the discharge current (A), △t refers to the discharge time (S), △ V represents the

potential difference (V), and m is the weight (g) of active material. As shown in Fig. 5A, B and C,

all the samples have approximately triangular charge/discharge curves and low IR drops at low current
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densities of 1 A g-1, indicating these materials had low contact resistance and transported ions quickly

42
. However, all the charge/discharge curves had a little curvature at a low current density of 1 A g-1

New Journal of Chemistry Accepted Manuscript

due to the surface oxygen groups deduced from the activation process 31. Fig. 6 shows the TPD curves

obtained of WBC-0, WBC-1, WBC-2 and WBC-3. As shown in Fig. 6, it can be observed that the
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amounts of CO of KOH-pretreated carbon materials are larger than the direct carbonized materials.

Indicating the carbon materials treated with KOH at high temperature under N2 atmosphere can

produce lots of oxygen-containing functional groups. With the increased amount of KOH, the number

of surface oxygen groups is a corresponding increase. This result indicates KOH is helpful to improve

the surface oxygen groups of carbon materials. So the high specific capacitance of WBCs could be due

to the abundant porosity with high specific surface area and oxygen-containing functional groups,

combining double-layer and Faradaic contributions. WBC-1, WBC-2 and WBC-3 showed specific

capacitance of 243, 268 and 186 F g-1 at the current density of 1 A g-1, respectively. The specific

capacitance slightly decreases with the increasing of the current density because of the inadequate time

for electrolyte diffusion 2. However, the specific capacitance of WBC-2 could still maintain 222 F g-1 at

a high current density of 10 A g-1, while the specific capacitance of WBC-1 and WBC-3 are 144 and

133 F g-1, respectively (Fig. 5D). This result might be due to the high specific surface, the pore size

distribution and some surface oxygen groups of the obtained carbon materials which had contributed to

transfer electrolyte ions conveniently.

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New Journal of Chemistry Accepted Manuscript

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Fig 5 Galvanostatic charge/discharge curves of WBC-1 (A), WBC-2 (B) and WBC-3 (C) at different

current densities; Specific capacitances of samples at different current densities (D).

Fig. 6 TPD curves of WBC-0, WBC-1, WBC-2 and WBC-3.

The electrochemical impedance spectroscopy (EIS) is further used to investigate the conductivity

of the electrode material. Fig. 7 shows the EIS spectrums of WBC-1, WBC-2 and WBC-3 in the

frequency range of 10-1-105 Hz. The theoretical Nyquist plot consists of two regions, (i) an irregular

semicircle at high frequency region and (ii) a straight line at low frequency region. As depicted in Fig.

7, the Nyquist plots are almost vertical lines at low frequency region, indicating a typical double-layer

charge storage behavior 43. The inset in Fig. 7 shows a well-defined semicircle at high frequency region

for WBC-2. The Nyquist plot is relatively 45o Warbury region, which is the typical feature of porous
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44, 45
carbon-based electrode . The semicircle at high frequency region is related to the charge transfer

resistance (Rct) of the electrode, which is induced by the electroactive surface area of the electrode 7.

New Journal of Chemistry Accepted Manuscript

The Rct of these samples are all very low, which could improve the ion transmission rate. The reduced

Rct of electrode materials is helpful to obtain better rate capability, because Rct is an important factor
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for fast charge and discharge of supercapacitors 46.

Fig. 7 Nyquist plots in the frequency range from 10-1 to 105 Hz.

Inset: magnified 9-14 Ω region.

Furthermore, the long-term cycle stability is one of the most crucial factors for supercapacitors.

The cyclic stability of WBC-2 was investigated by using galvanostatic charge and discharge technique

at a current density of 10 A g-1 in 6 M KOH electrolyte for 5000 cycles. Fig. 8 shows the retention of

specific capacitance with cycle number. The specific capacitance is reduced obviously between 0 and

1500 cycles and retained up to 2500 cycles. It retains 97.28 % of the initial specific capacitance after

5000 cycles. The dropping in the specific capacitance could be on account of irreversible reaction

47
between electrode and electrolyte . As shown in the inset in Fig. 8, the charging and discharging

curve of the sample is completely symmetrical due to the high specific surface area and abundant

porosity. This result indicates that WBC-2 electrode shows an excellent stability in cyclic

charge/discharge process because of its large specific surface, extensively micropore structure and high
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graphitic degree.

New Journal of Chemistry Accepted Manuscript

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Fig. 8 Cycle stability of WBC-2 at constant current density of 10 A g-1 for 5000 cycles.

Inset: galvanostatic in charge/discharge cycles.

4. Conclusion

In summary, three porous carbon materials with tunable microstructures were successfully

prepared via carbonization of KOH-pretreated water bamboo through adjusting the rations of KOH.

Based on the experimental results, the porous carbon material synthesized at 2:1 weight ratio of KOH

to water bamboo-derived carbon exhibited a high specific capacitance of 268 F g-1 in 6 M KOH

electrolyte at a current density of 1 A g-1 and retained up to 222 F g-1 even at a current density of 10 A

g-1. In addition, these materials also showed excellent capacity retention of 97.28 % over 5000 cycles at

a current density of 10 A g-1. All of the above results demonstrated that the electrochemical properties

of water bamboo-derived carbon-based electrodes could be affected by specific surface area, pore size

distribution and pore volume. While abundant micropores could increase the specific capacitance area,

the existence of mesopores contributed to the efficiently movement of electrolyte ions and obtain high

electrochemical performance. The excess amount of KOH could lead to collapse of the micropore

volume and the pore structure, which reduced the conductivity of material and further affected its

electrochemical performance. In summary, microporous carbon materials can be easily synthesized

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from natural plant water bamboo for as an ideal electrode material for supercapacitors.

Acknowledgements

New Journal of Chemistry Accepted Manuscript

The authors are grateful to the financial support of the National Natural Science Foundation of

China (Nos. 21471114, 91122025, 21103127, 21101118), the State Major Research Plan (973) of China
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(No. 2011CB932404), and the Nano-Foundation of Shanghai in China (No. 11nm0501300).

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