Journal of Cleaner Production 236 (2019) 117692

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Journal of Cleaner Production

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

Cleaner conversion of bamboo into carbon fibre with favourable

physicochemical and capacitive properties via microwave pyrolysis
combining with solvent extraction and chemical impregnation
Su Shiung Lam a, b, *, 1, Elfina Azwar b, 1, Wanxi Peng a, 1, Yiu Fai Tsang c, 1, Nyuk Ling Ma d, 1,
Zhenling Liu e, Young-Kwon Park f, Eilhann E. Kwon g, **
a
School of Forestry, Henan Agricultural University, Zhengzhou, 450002, China
b
Pyrolysis Technology Research Group, School of Ocean Engineering, Universiti Malaysia Terengganu, 21030 Kuala Terengganu, Terengganu, Malaysia
c
Department of Science and Environmental Studies, The Education University of Hong Kong, Tai Po, New Territories, Hong Kong
d
School of Fundamental Science, Universiti Malaysia Terengganu, 21030, Kuala Terengganu, Terengganu, Malaysia
e
School of Management, Henan University of Technology, Zhengzhou, 450001, China
f
School of Environmental Engineering, University of Seoul, Seoul, 02504, Republic of Korea
g
Department of Environment and Energy, Sejong University, Seoul, 05005, Republic of Korea

a r t i c l e i n f o a b s t r a c t

Article history: Bamboo was converted into carbon fibre using a novel approach combining microwave pyrolysis, solvent
Received 12 February 2019 extraction, and chemical impregnation. The employment of solvent extraction and chemical impreg-
Received in revised form nation transformed natural bamboo into bamboo fibre with yield of 64 wt% that comprised of 87 wt%
13 July 2019
cellulose, 4 wt% lignin and 9 wt% hemicellulose deemed desirable for conversion into carbon fibre. The
Accepted 15 July 2019
Available online 16 July 2019
subsequent use of microwave pyrolysis transformed the bamboo fibre to form carbon fibre; the effects of
microwave irradiation time and microwave power (two key process parameters) on properties of carbon
Handling editor. Charbel Jose Chiappetta fibre were investigated. Microwave pyrolysis provides a rapid heating rate (30
C/min) with relatively
Jabbour shorter process time (20 min) compared to that performed by conventional pyrolysis method, thus
leading to a relatively lower electric consumption and providing a potentially cost-saving and energy-
Keywords: efficient approach to produce carbon fibre. The production and properties of carbon fibre produced
Pyrolysis were affected by irradiation time and microwave power. The carbon fibre obtained was detected to have
Microwave high fixed carbon (80 wt%), carbon element (87%), high BET surface area (475 m2/g) and fibres in small
Bamboo
diameter (1 mm). It also shows desirable features comprising low content of moisture (<6 wt%), inor-
Carbon fibre
ganic elements of Na, K, S, Mg (5%) and ash (1 wt%), allowing the carbon fibre to have more active sites
Energy
and making it a cleaner product rather than polluting the environment whereas a high ash content could
lead to undesired catalytic reactions and emission of potentially hazardous metallic components present
in the ash. Combined with the detection of positive capacitive behaviour, the carbon fibre shows great
potential to be used as an electrode for energy storage application. The results disclose that microwave
pyrolysis combining with solvent extraction and chemical impregnation can be a cleaner approach to
transform bamboo into carbon fibre with favourable physicochemical and capacitive properties.
© 2019 Elsevier Ltd. All rights reserved.

1. Introduction

Bamboo is a biomass that is abundantly available as a global

forest resource which accounts for approximately 15 million tons of
* Corresponding author. School of Forestry, Henan Agricultural University, annual production over 1200 species (Liu et al., 2016), owing to its
Zhengzhou, 450002, China. fast growth (Peng et al., 2013), abundant availability, being
** Corresponding author. renewable and eco-friendly source, making it favourable for use as
E-mail addresses: lam@umt.edu.my (S.S. Lam), ekwon74@sejong.ac.kr feedstock in various applications (Jayanetti and Follett, 2008) and
(E.E. Kwon).
1
These authors contributed equally to this paper and act as first authors.
short maturity period (Li et al., 2012). Recently, efforts on

https://doi.org/10.1016/j.jclepro.2019.117692
0959-6526/© 2019 Elsevier Ltd. All rights reserved.
2 S.S. Lam et al. / Journal of Cleaner Production 236 (2019) 117692
employing bamboo in energy storage applications have been
studied, which reported that bamboo-based carbon fibre shows
potential for use as electrode material in energy storage application
(Yang et al., 2018b).
Carbon fibre is a different type of carbon-based material
compared to activated carbon (Wong et al., 2016), char, carbon
microsphere, carbon nanotube (Ko € hler et al., 2008), graphene and
graphene quantum dot (Safardoust-Hojaghan and Salavati-Niasari,
2017). Carbon fibre has a distinct surface morphology of fibrous,
thread-like with cup-stacked structure and low density that can be
applied in processing parts of cellular phones, laptops, portable
devices and electric vehicles (Kong et al., 2017; Zhang et al., 2016). It
can be altered to form nanostructures (i.e carbon nanofibres) that
can generate quantum effects at nano-scale (Azwar et al., 2018).
Despite of its advantages and diverse applications, carbon fibre
is often claimed as an expensive material due to high precursor cost
and amount of energy needed to heat the fibres (Das, 2011).
Hermansson et al. (2019) revealed that the use of common pre-
cursors such as carbon fibre reinforced polymer (e.g poly-
acrylonitrile) with conventional heating need high operating
temperature (1700
C) and can pollute the environment through
emissions of air pollutants such as ammonia and hydrogen cyanide.
Furthermore, polyacrylonitrile is derived from non-renewable and
relatively expensive petroleum that has contributed up to 50% of
carbon fibre manufacturing cost (Yang et al., 2013). For this reason,
efforts have been made to find an alternative of cheaper, eco-
friendly and renewable carbon fibre precursor. It is reported that
the use biomass-based material such as lignin can reduce the
precursor cost, energy consumption and CO2 equivalent green-
house emission by 22%, 5% and 13% compared to polyacrylonitrile
precursor (Das, 2011).
Carbon fibre, being a promising carbon-based material can be
synthesized by several techniques, namely, pyrolysis (Kim et al.,
2017), electrospinning (Beck et al., 2017), hydrothermal treatment
(Deng et al., 2017), ultrasonication (Liu et al., 2017a) and chemical
vapour deposition (Liu et al., 2017b). (Liu et al., 2017b). These
techniques have their own pros and cons where they were
employed to achieve different objectives, either to achieve high
product yield, adjustment of feasible diameter, low electric con-
sumption, or shorter production time. Interestingly, pyrolysis has
been reported as a potential approach that enables mass produc-
tion of biomass-based carbon fibre compared to other techniques
(Lee et al., 2017). Although pyrolysis is less advantageous in
tailoring the carbon fibre diameter compared to electrospinning, it
does not require additional carbonisation step for post treatment
(Azwar et al., 2018).
Pyrolysis is an approach that can breakdown biomass thermally
in inert condition to yield pyrolysis products (i.e carbon rich resi-
dues, incondensable gas and liquid oil) (Liew et al., 2018a). None-
theless, conventional pyrolysis commonly employs energy-
intensive and non-selective heating sources such as furnace that
require long process time to achieve target process temperature
(approximately 700
C). The heating coil of furnace supplies heat
energy, targeting the entire chamber through conduction and
convection mechanisms. As a result, longer process time (>2 h) is
needed to heat up the sample until desired temperature is achieved
(Lam et al., 2017; Liew et al., 2018b). On the contrary, microwave
pyrolysis provides rapid process time as it employs microwave ra-
diation mechanism that could induce rapid dipole rotation within
the biomass material (Yek et al., 2019). The dipole rotation of the
molecules in biomass material could generate frictions and in turn
heat up in a shorter time. Liew et al. (2019) had revealed that mi-
crowave pyrolysis can be an alternative for sustainable and efficient
approach for biomass conversion into valuable products as it pro-
vides higher heating rate (60
C/min), fast process time (35 min)
and lower energy consumption (1470 kJ) compared to furnace-
assisted pyrolysis (2e10
C/min; 4 h; 61920 kJ), thus reducing
manpower and operating costs (Liew et al., 2018b).
Most studies on pyrolysis of bamboo only focused on conven-
tional pyrolysis conversion of bamboo into common products such
as char (Hernandez-Mena et al., 2014; Huff et al., 2014; Liu et al.,
2014; Sun et al., 2014) and bio-oil (Chen et al., 2014; Jung et al.,
2008; Miao et al., 2007; Yi et al., 2012). To the best of our knowl-
edge, there are limited studies reported on the transformation of
bamboo into carbon fibre using microwave pyrolysis. Herein, we
demonstrate the employment of a cleaner approach by combining
microwave pyrolysis, solvent extraction, and chemical impregna-
tion techniques to transform bamboo into carbon fibre. This study
aims to develop an approach with improved efficiencies in energy
consumption and human capital, and preventing the emission of
hazardous gases. In this study, microwave pyrolysis of bamboo was
examined over a range of microwave power (600e800 W) and
irradiation time (20e40 min) with emphasis on physicochemical
properties (i.e proximate content, elemental content, chemical
functional groups, surface morphology and porous characteristics)
and capacitive behaviour of carbon fibre. This study aims to develop
a cleaner approach to convert bamboo into carbon fibre for po-
tential use in energy storage application.
2. Material and methods
2.1. Transformation of raw bamboo into carbon fibre
Raw bamboo (Phyllostchys edulis) was obtained from a local
bamboo farm in Kampung Gong Badak, Terengganu, Malaysia. The
raw bamboo was cut into ring-shaped (1 cm thick) using metal
horizontal bandsaw (23 cm in width x 41 cm in length). This was
followed by cutting of raw bamboo into cube-shaped (1 cm in
width x 1 cm in length x 1 cm in height) using scissor. After that, the
raw bamboo was cleaned using distilled water and then dried for
24 h at 110
C to ensure all physically bound moisture were
removed from bamboo surface (Anisuzzaman et al., 2016). The
dried raw bamboo was kept in a plastic container prior to any
analysis.
60 g of raw bamboo was extracted with a mixture of ethanol and
0.5 M of sulphuric acid at a volume ratio of 1:10 for 6 h using
soxhlet extraction to remove resins, fats, wax and phenolic ex-
tractives (Conrad, 1944; Eberhardt et al., 2006). The changes in
chemical composition of raw bamboo were tabulated in Table 1. The
lignin in the treated bamboo was then removed via treatment with
1.3 wt% of acidified sodium chlorite (NaClO2) for 1 h at 90
C. The
acidification of sodium chlorite was done by adding few drops of
acetic acid until pH 4 was achieved. The treated bamboo was
filtered and washed with 1 wt% of sodium hydroxide (NaOH) to
remove excess acidified NaClO2. Then, the treated bamboo was
impregnated with 5 wt% of potassium hydroxide (KOH) at 80
C for
6 h to remove hemicellulose, thus producing bamboo fibre. The
bamboo fibre was filtered and washed with 1 wt% of HCl to remove
excess KOH. The bamboo fibre was then rinsed with distilled water
Table 1
Chemical composition of raw bamboo and bamboo fibre.
Content (wt%) Raw bamboo Bamboo fibre
Extractive 3.10 e
Lignin 22.50 3.56
Acid insoluble lignin 21.17 0.62
Acid soluble lignin 1.33 2.94
Hemicellulose 30.53 9.12
Cellulose 43.88 87.32
 S.S. Lam et al. / Journal of Cleaner Production 236 (2019) 117692
until the pH was neutral. The bamboo fibre was dried for 2 days at
80
C. A yield of 50 wt% bamboo fibre was obtained then kept in a
closed jar prior to microwave pyrolysis.
Microwave pyrolysis was chosen to convert the bamboo fibre
into carbon fibre via a pyrolysis set up that had been proposed by
Lam et al. (2017a). Approximately, 2 g of bamboo fibre and 15 g of
coconut-based activated carbon (Kekwa Indah Sdn Bhd, Malaysia)
were inserted into a pyrolysis reactor that was then placed into a
microwave oven. Activated carbon was applied as microwave
absorber to absorb microwave radiation and in turn heated up the
entire pyrolysis system. It also enhanced the heat transfer to the
bamboo fibre in order for extensive pyrolysis cracking of the
bamboo fibre to occur (Mene ndez et al., 2010). An inert condition is
set up by purging nitrogen gas through the pyrolysis reactor at a
flow rate of 0.25 L/min while a thermocouple (K-type) was chosen
to assist the temperature of the reactor. Different microwave
powers (600e800 W) were adjusted for 30 min to pyrolyze and
convert bamboo fibre to form carbon fibre (CF). The CF obtained
was separated from activated carbon using stainless steel tweezer
and labelled as ‘CF600’, ‘CF700’ and ‘CF800’ where the number of
600, 700, and 800 refers to the respective microwave power. The
microwave pyrolysis method was repeated over a range of irradi-
ation time (20e40 min) at 700 W and labelled according to their
respective irradiation time as ‘CF20’, ‘CF30’ and ‘CF40’.
2.2. Characterization of raw bamboo, bamboo fibre and carbon
fibre
Thermogravimetric analysis (TGA) using a Mettler Toledo TGA
analyser was performed to examine the stages of decomposition
occurred during pyrolysis of the raw bamboo as well as proximate
content (ash, fixed carbon, moisture, volatile matter) of the raw
bamboo, bamboo fibre and carbon fibre. The TGA was conducted by
heating the samples at a heating rate of 10
C/min from 30 to 950
C
with nitrogen gas (N2) as carrier gas. The samples were pyrolyzed in
N2 environment with a gas flow rate of 50 mL/min. The moisture
and volatile matter content of the samples were determined by
weight loss from TGA curve at 110
C and between 150 and 450
C
respectively. The combustion at 950
C for 20 min using a muffle
furnace was conducted to determine the ash content, while the
fixed carbon content was obtained by subtracting the original dry
mass of sample with ash, moisture and volatile matter content.
The chemical composition was obtained according to method
from Adeeyo et al. (2015). Firstly, 2.5 g of dried sample was
extracted using 150 mL of acetone at 70
C for 4 h. The sample was
air dried at room temperature for few minutes followed by drying
using oven at 105
C. The extractives content was evaluated as the
difference in weight. Then, 1 g of extracted sample was added into
150 mL of 500 mol/m3 NaOH followed by boiling for 3.5 h. The
mixture was filtered after cooling through vacuum filtration and
washed until neutral pH. The residue was dried to a constant
weight at 105
C in a convection oven. The hemicellulose was
calculated by difference between the sample weight before and
after this treatment. The lignin content was measured by adding
3 mL of 72% H2SO4 into 0.3 g of dried extracted sample. The sample
was shaking for 30 min to allow for complete hydrolysis. After that,
84 mL of distilled water was added and autoclaved for 1 h at 121
C.
The mixture was filtered through vacuum using a filtering crucible.
The acid insoluble lignin was determined by drying the residues at
105
C and accounting for ash by incinerating the residues at 575
C
in a muffle furnace. The acid soluble lignin fraction was determined
by measuring the absorbance of the acid hydrolyzed samples at
320 nm. The lignin content was calculated as the summation of acid
insoluble lignin and acid soluble lignin. The cellulose content was
calculated by difference, assuming that extractives, hemicellulose,
3
lignin, ash, and cellulose are the only components of the entire
biomass.
SEM-EDX (JEOL JSM-6360LA) was used to determine the surface
morphology and elemental content of samples at 10 kV of accel-
erating voltage. The elemental analysis of samples were also per-
formed using FlashEA 1112 CHNS elemental analyser to quantify the
carbon, hydrogen, nitrogen and sulphur contents. Fourier trans-
form infrared spectra (FTIR) (Perkin Elmer Spectrum 100) were
performed to analyse the chemical functional groups in the sam-
ples at spectra from 400 to 4000 cm1. The FTIR sample was pre-
pared by mixing with potassium bromide (ratio 1:7) using pestle
and mortar. The X-ray diffraction patterns of samples were
observed on a Ultima III diffractometer with CuK f radiation
(l ¼ 1.5406 Å) to explore the changes of phase structure of samples.
Brunauer-Emmett-Teller (BET), Barrett, Joyner and Halenda (BJH)
and t-plot method were employed using nitrogen adsorption-
desorption isotherm (Micromeritics, ASAP, 2010) to determine
specific surface area, total pore volume and average pore size of
samples.
2.3. Capacitive behaviour of carbon fibre
Cyclic voltammetry (CV) is an effective electrochemical test to
reveal the capacitive behaviour of a given material. Cyclic voltam-
metry (Potentiostat Galvanostat, Autolab PGSTAT) was carried out
using a three-electrode set up (working electrode, counter elec-
trode and reference electrode). The working electrode, counter
electrode and reference electrode were made from carbon fibre,
saturated calomel and platinum material. The carbon fibre elec-
trodes were fabricated from carbon fibre using a slurry coating
method. The carbon fibre obtained was adhered using poly(methyl
methacrylate)(PMMA) with a mass ratio of 90:10. The mixture of
carbon fibre and PMMA was dissolved using ethyl acetate to form
ink-like slurry. The slurry was then coated on an aluminium foil
with an area of 1 cm in width x 1 cm in length. The coated
aluminium foil was dried at 100
C for one night. The CV was set up
by dipping the all electrodes in 1 M of KNO3 electrolyte with po-
tential difference (DV) of 0.8 V by adjusting the potential supplied
(V) from 1.0 to 1.8 V.
3. Results and discussion
3.1. Characterization of raw bamboo and bamboo fibre as a
feedstock for microwave pyrolysis
The pyrolytic behaviour of bamboo materials (i.e raw bamboo
and bamboo fibre) were observed on TGA curve presented in Fig. 1.
The TGA curve shows the weight loss of bamboo materials as a
function of temperature. There were three decomposition stages of
bamboo materials observed during pyrolysis, namely: 1) evapora-
tion of moisture, 2) de-volatilisation of lignocellulosic component
and 3) carbonisation of non-volatile fraction. Initially, weight loss of
bamboo materials were observed from ambient temperature
(30
C) up to 110
C. The weight loss was likely to be derived from
evaporation of water (moisture) physically bound on the surface of
bamboo (Dubey et al., 2018). Then, the bamboo materials experi-
enced a drastic weight loss at temperature between 150 and 450
C.
This can be attributed to the de-volatilisation of lignocellulosic
component (Nam et al., 2018).
The lignocellulosic component present within bamboo mate-
rials comprised mainly hemicellulose, cellulose and lignin, which
had been reported to have varying thermal stability which would
break down at different temperature ranges (Cheng et al., 2015).
During the de-volatilisation of lignocellulosic component, a weight
loss of bamboo materials can be observed at a lower temperature
4 S.S. Lam et al. / Journal of Cleaner Production 236 (2019) 117692
Fig. 1. TGA curve of raw bamboo and bamboo fibre.
between 150 and 285
C. This could be attributed to decomposition
of hemicellulose as it has the lowest thermal stability compared to
other lignocellulosic component (i.e cellulose and lignin). Hemi-
cellulose is a heteropolysaccharide (a carbohydrate that is made
from different monomer types) typically made from simple units of
xylan, arabino-xylan and gluco-mannan connected with b-1,3
glycosidic bonds (Aristidou and Penttila €, 2000), thus resulting in a
lower degree of polymerisation (less than 200 kDa), structural
stability and activation energy (i.e minimum energy required to
break chemical bonds) (Pe rez et al., 2018). Consequently, heating at
a relatively low temperature is sufficient to overcome the lower
degree of polymerisation, structural stability and activation energy
of hemicellulose. This explains the lowest thermal stability of
hemicellulose compared to cellulose and lignin. A little weight loss
of bamboo fibre at this temperature range indicates its low hemi-
cellulose content compared to raw bamboo, suggesting more
hemicellulose had been removed during chemical impregnation.
At a higher temperature of de-volatilisation between 285 and
365
C, the weight loss of bamboo materials could be due to the
decomposition of cellulose. Cellulose is a homopolysaccharide
(carbohydrates that is made from one monomer type) of repeating
glucose molecules linked by b-1,4 glycosidic bonds to form glucan
chains (Yang et al., 2007). The glucan chains of cellulose are usually
connected by hydrogen bonds to form highly ordered microfibrils,
thus making cellulose stronger than hemicellulose. This could
explain the decomposition of cellulose of bamboo materials at a
higher pyrolysis temperature than hemicellulose.
The weight loss during de-volatilisation between 365 and
500
C may be due to the lignin decomposition. Lignin, having the
most thermally stable and complex structure compared to other
lignocellulosic component of bamboo (Kan et al., 2016; Liew et al.,
2018b), is made from phenolic polymers that consist of three types
of phenylpropane units (i.e p-coumaryl alcohol, coniferyl alcohol,
and sinapyl alcohol) linked by strong ether and carbon-carbon
linkages (Bugg et al., 2011). The presence of complex structure
and strong linkages had caused the need of higher temperature to
decompose lignin, thus explaining the highest thermal stability of
lignin compared with other lignocelluosic materials. The bamboo
fibre also shows lesser weight loss at this temperature range
compared to raw bamboo, indicating lesser lignin content have
been removed during chemical impregnation.
From the TGA curve, it can be noticed that the bamboo materials
showed a nearly constant rate of weight loss from 500
C onwards.
This is due to lower release of lower molecular weight carbon
species and incondensable gases while leaving non-volatile fixed
carbon to be remained as the solid product. This indicates that the
thermochemical decomposition of bamboo materials was almost
complete at this temperature. It is thus suggested that a minimum
temperature of 500
C is needed to carbonise/pyrolyze bamboo
materials in producing carbon-rich solid product such as carbon
fibre that is potentially desirable for use in applications such as
waste adsorption treatment and energy storage.
3.2. Yield of carbon fibre microwave pyrolysis
Fig. 2 displays the yield of carbon fibre at varying irradiation
time and microwave power of microwave pyrolysis. Initially,
64.27 wt% of bamboo fibre was obtained after soxhlet extraction
and chemical impregnation of bamboo. After microwave pyrolysis,
carbon fibre was obtained with a yield of up to 13.11 wt% and
heating rate of 30
C/min as observed from the temperature
monitor. It can also be observed that carbon fibre produced at
longer irradiation time (40 min) and higher microwave power
(800 W) produced lower yields (9.93e10.95 wt%) whereas higher
yields (12.88e13.11 wt%) were obtained at lower irradiation time
and microwave power.
The higher amount of microwave radiation produced at higher
microwave power has increased the extent of rapid dipole rotation
of covalent bonds within bamboo fibre particles. Combined with
prolonged irradiation time, this increased the extent of dipole
rotation and friction forces between bamboo fibre particles, thus
producing more heat inside the bamboo fibre and resulting in
extensive pyrolysis conversion of bamboo fibre to produce volatile
matter. Consequently, more volatile matter was emitted from the
bamboo fibre, resulting in formation of a lower amount of carbon
fibre as the solid product in the reactor. On the other hand, the
higher yield of carbon fibre produced at shorter irradiation time
and lower microwave power was due to less generation of heat and
decrease in release of volatile matter during microwave pyrolysis.
3.3. Characterization of raw bamboo, bamboo fibre and carbon
fibre
The proximate and elemental contents of raw bamboo, bamboo
 S.S. Lam et al. / Journal of Cleaner Production 236 (2019) 117692 5

Fig. 2. Yield of bamboo fibre and carbon fibre.

fibre and carbon fibre produced at different irradiation time and content lead to undesired catalytic reaction occurred during the use
microwave power are tabulated in Table 2 and Table 3 respectively. of the carbon fibre as catalyst in high temperature applications such
The carbon fibre obtained consists of higher fixed carbon content as pyrolysis process (700e900
C) (Liew et al., 2018a); carbon
(61e80 wt%) and lower contents of moisture (4e6 wt%), volatile products have been used as base material to form catalyst via
matter (13e33 wt%) and ash (1 wt%) compared to raw bamboo and impregnation with metals. This could in turn result in emission of
bamboo fibre. potentially hazardous metallic components present in the ash.
The low moisture content (4e6 wt%) detected for carbon fibre It is found that carbon fibre produced at longest irradiation time
can be a beneficial feature to determine its feasibility as a feedstock (CF40) and highest microwave power (CF800) had the highest fixed
for use in agricultural and manufacturing industries (Liew et al., carbon content (78e80 wt%) and lowest volatile matter content
2018a; Tomar et al., 2017). This is because biomass generally con- (13e15 wt%). This was likely because the higher microwave power
tains a high moisture content (up to 90 wt%) that needs to be (800 W) and longer irradiation time (40 min) during microwave
removed to reduce the rate of biological deterioration and maxi- pyrolysis had transferred more microwave energy to the bamboo.
mise its bulk density for transportation to factory or treatment More heat energy were generated within the bamboo fibre, leading
facilities (Tomar et al., 2017). Consequently, there is an additional to the enhancement of pyrolysis decomposition of bamboo fibre to
cost required for drying of biomass feedstock prior to any pro- produce and release more volatile matter, resulting in formation of
cessing steps. Therefore, carbon fibre with low moisture content carbon fibre with higher non-volatile component, i.e fixed carbon,
can be considered as an economical feasible feedstock due to the compared to raw bamboo and bamboo fibre.
less electric consumption and the resulting cost required for drying. In contrast, the carbon fibre produced at the lowest microwave
Low content of ash and moisture are also always favourable because power (CF600) and shortest irradiation time (CF20) showed the
the presence of moisture tends to block the active sites, thus lowest fixed carbon content (61e70 wt%) and highest volatile
influencing the functionality of carbon fibre, while a high ash matter content (25e33 wt%). This suggests that the heat energy
generated at 600 W and 20 min duration of irradiation were not
sufficient to pyrolyze and carbonise the bamboo fibre, thus pro-
Table 2 ducing carbon fibre with lower fixed carbon content and higher
Proximate content of raw bamboo, bamboo fibre and carbon fibre. volatile matter content. Therefore, the irradiation time and micro-
wave power of microwave pyrolysis were deemed to have a sig-
Proximate content (wt%) Moisture Volatile matter Fixed carbon Ash
nificant effect on the proximate content of carbon fibre obtained.
Raw bamboo 7 65 26 2 The carbon fibre was detected to be dominated by higher carbon
Bamboo fibre 5 75 17 3
CF20a 4 25 70 1
content (80.1e87.2%) compared to raw bamboo and bamboo fibre.
CF30a 6 17 76 1 This could be attributed to the impregnation of bamboo fibre using
CF40a 6 15 78 1 KOH. During KOH treatment, the OH ions derived from KOH
CF600b 5 33 61 1 would attack the chemical bond across oxygen and carbon atoms.
CF700b 6 17 76 1
More advanced irradiation time and microwave power had thus
CF800b 6 13 80 1
weakened and broke more chemical bond between oxygen and
a
Carbon fibre obtained at different irradiation time (20, 30, 40 min). carbon atoms present in the bamboo fibre, thus releasing more
b
Carbon fibre obtained at different microwave power (600, 700, 800 W).
6 S.S. Lam et al. / Journal of Cleaner Production 236 (2019) 117692

Table 3
Elemental content of raw bamboo, bamboo fibre and carbon fibre.

Elemental content (%) Cc Hc Nc Sc Oe Cd Od Nad Md Sid Sd Cld Kd

Raw bamboo 41.5 6.1 0.7 0.0 51.7 45.7 51.6 0.1 0.0 0.3 0.1 0.0 0.0
Bamboo fibre 58.2 5.1 0.6 0.0 36.1 53.7 36.3 0.1 0.0 0.0 0.0 3.8 5.9
CF20a 80.1 4.5 0.5 0.0 14.9 92.6 1.6 0.5 0.0 0.0 0.0 1.7 3.1
CF30a 84.4 3.9 0.3 0.0 11.4 97.3 0.6 0.3 0.0 0.0 0.0 0.9 0.7
CF40a 86.5 3.1 0.2 0.0 10.2 97.4 0.5 0.3 0.0 0.0 0.0 0.5 0.7
CF600b 81.7 4.6 0.5 0.0 13.2 90.9 1.4 0.1 0.0 0.0 0.0 1.9 5.4
CF700b 84.4 3.9 0.3 0.0 11.4 97.3 0.6 0.3 0.0 0.0 0.0 0.5 0.7
CF800b 87.2 2.4 0.1 0.0 10.3 98.3 0.5 0.0 0.0 0.0 0.0 0.4 0.0
a
Carbon fibre obtained at different irradiation time (20, 30, 40 min).
b
Carbon fibre obtained at different microwave power (600, 700, 800 W).
c
Data obtained from CHNS analyser.
d
Data obtained from EDX analyser.
e
Obtained by difference (100-C-H-N-S).

oxygenated component from bamboo fibre. This explained the ef-

fect of irradiation time and microwave power on carbon and oxy-
gen content of carbon fibre. The high carbon content is always
desirable as it can improve the capacitive properties of carbon fibre.
This is because carbon element could be arranged in a sp2 structure
that could provide a delocalized pi-bond and free charge carrier,
thus facilitating the electrical properties of carbon fibre (Gu et al.,
2015; Pandolfo and Hollenkamp, 2006).
Small amount of Na element (up to 0.5%) was observed within
the carbon fibre obtained. This could be derived from the Na resi-
dues remained on carbon fibre surface after the washing step with
NaOH. The presence of K element (up to 5.4%) and Cl element (up to
1.9%) can be explained by the residues remained on carbon fibre
surface after metal hydroxide treatment (i.e KOH impregnation)
and post treatment (i.e HCl). However, the content of the Na, K and
Cl elements had decreased at longer irradiation time and higher
microwave power. This is due to the increase of evaporation and
removal of these residues from carbon fibre resulted from higher
heat energy produced at longer irradiation time and higher mi-
crowave power.
Fig. 3 presents the FTIR spectra of raw bamboo, bamboo fibre
and carbon fibre over a range of irradiation time and microwave
power. It can be observed that most of the carbon fibre had pro-
duced almost similar FTIR peaks at different levels of transmittance.
An absorption band of FTIR of carbon fibre between 3200 and
3600 cm1 corresponds to the OeH stretching of carboxyl, phenol
or alcohol group (Yakout and Sharaf El-Deen, 2016). The small band
at about 1670e1760 cm1 was corresponded to C¼O stretching
vibrations of carboxyl groups, ketones, lactones or aldehydes. The Fig. 3. FTIR spectra of raw bamboo, bamboo fibre and carbon fibre over varying mi-
crowave power (a) and irradiation time (b).
FTIR spectrum of the carbon fibre also showed a strong band at
1530e1670 cm1 due to presence of compounds with aromatic ring
group, and the weak band at 1380-1450 cm1 indicated compound Fig. 4 shows the XRD patterns of raw bamboo, bamboo fibre and
with CeH bending (alkane). Several functional groups of carbon carbon fibre obtained over a range of irradiation time and micro-
fibre such as CH2, CeH and OeH that represent alkene, alkane and wave power. It can be observed that raw bamboo, bamboo fibre and
phenol can be detected at absorption band of 1280e1380 cm1. The carbon fibre have a broad peak at 2q ¼ 21.7
, which corresponds to
peaks at frequency ranging between 1180 and 1280 cm1 and (002) plane of amorphous carbon of lignocellulosic compounds. A
900e1180 cm1 were assigned to OeH bending and CeO stretching weak peak at 2q ¼ 24.3
was also noticed for all samples, suggesting
in esters, ethers, alcohols and/or phenols groups (Yakout and Sharaf the presence of crystalline structure arranged in stacked layers. It
El-Deen, 2016). was observed that the broad peak at 2q ¼ 21.7
and the weak peak
It can also be noticed from FTIR analysis that weaker peaks at 2q ¼ 24.3
of carbon fibre obtained from microwave pyrolysis of
(peaks with lower intensity of infrared absorption) were detected bamboo become sharper with higher intensity compared to that
for carbon fibre obtained over longer irradiation time and higher observed for raw bamboo and bamboo fibre, suggesting that the
microwave power. This was likely due to the extensive breaking of microwave pyrolysis process had caused changes to the amorphous
chemical bonds within the complex structure of carbon fibre at structure of lignocellulosic compound originally present in
longer irradiation time and higher microwave power. As a result, bamboo, transforming some of the lignocellulosic compounds to
many functional groups were removed during microwave pyrolysis form more stable and crystalline cellulose II (Ronald Aseer et al.,
that in turn formed simpler structure of carbon fibre, thus 2013). The peak of carbon fibre at 2q ¼ 24.3
become sharper at
explaining the low intensity FTIR peaks. longer irradiation time and higher microwave power, indicating
 S.S. Lam et al. / Journal of Cleaner Production 236 (2019) 117692
Fig. 4. XRD patterns of raw bamboo, bamboo fibre and carbon fibre over varying microwave power (a) and irradiation time (b).
that more crystalline carbon structure had been formed in carbon
fibre (Gu et al., 2015). The presence of more crystalline structure at
longer irradiation time (40 min) can be explained by the sufficient
duration for rearrangement of irregular cellulose I into crystalline
cellulose II (Ben Sghaier et al., 2012). Interestingly, graphitic planes
(100,101) commonly found in carbonaceous materials near
2q ¼ 43
were not detected for the carbon fibres produced in this
study. This can be explained by chemical impregnation that was
likely to have broken the (100,101) planes, thus destroying the
orderliness in atomic arrangement of these planes (Yang et al.,
2014; Zhang et al., 2018).
The more advanced microwave power (800 W) also had facili-
tated the formation of turbostratic structure of carbon, a graphite-
like microcrystallite stacked in nearly parallel layers. This is because
more heat energy were obtained to break down and rearrange
(002) plane of amorphous carbon into more crystalline and ordered
layers (Gu et al., 2015). Therefore, the results suggest that the phase
structure of carbon fibre can be improved to form a more crystalline
structure by adjusting the irradiation time and microwave power of
microwave pyrolysis. Carbon fibre with more crystalline structure
is desirable as it is stronger and stiffer than amorphous structure,
thus improving its mechanical strength for use in many
applications.
The porous characteristics (pore size distribution, total pore
volume and BET surface area) of raw bamboo, bamboo fibre and
carbon fibre obtained at different irradiation time and microwave
powers are tabulated in Table 4. It can be noticed that the BET
surface area of carbon fibre was increased from 83 up to 475 m2/g
and the total pore volume was increased from 0.07 up to 0.24 cm3/g
at increasing irradiation time (20e40 min) and microwave power
(400e800 W) during microwave pyrolysis. The higher BET surface
7
area and total pore volume of carbon fibre could be explained by
the increased presence of microcrystallites (confirmed in XRD
pattern) and pores (confirmed using BJH and t-plot method) in
carbon fibre. The carbon fibre with higher BET surface area and total
pore volume is highly desirable as it could provide more active sites
for the transportation of charged ions onto carbon fibre surface
during energy storage application (Gu et al., 2015).
It was found that CF800 has the highest BET surface area
(475 m2/g) and total pore volume (0.24 cm3/g). The production of
CF800 with high pore volume was due to the KOH impregnation
followed by microwave pyrolysis at high microwave power
(800 W). During impregnation of bamboo fibre with KOH, reduc-
tion and oxidation occurred simultaneously (i.e redox reaction).
Initially, the KOH was dissociated into basic and reactive H2O and
K2O (Eq. (1)). The basic and reactive H2O derived from KOH was
then reacted with bamboo fibre, reducing H2O to H2 gas while the C
element from bamboo fibre was oxidized into CO (Eq. (2)). Then, the
CO adhered on bamboo fibre surface was removed in the form of
CO2 volatiles during the impregnation KOH at 90
C (Eq. (3)). The
K2O reacted with CO2 to form salt of K2CO3 (Eq. (4)) which was then
removed during washing step using distilled water. The main
mechanism of KOH treatment could be summarized as follows:
2KOH / H2 O þ K2 O (1)
C þ H2 O/CO þ H2 (2)
CO þ H2 O/CO2 þ H2 (3)
K2 O þ CO2 /K2 CO3 (4)
8 S.S. Lam et al. / Journal of Cleaner Production 236 (2019) 117692

Table 4
Porous characteristics of raw bamboo, bamboo fibre and carbon fibre.

Sample Average pore size (nm)c Total pore volume (cm3/g)d Micropore volume (cm3/g)e Mesopore volume (cm3/g)f BET surface area (m2/g)g

Raw bamboo 4.67 0.07 0.03 0.04 83

Bamboo fibre 3.8 0.08 0.01 0.06 104
CF20a 3.84 0.1 0.03 0.06 162
CF30 a 3.71 0.15 0.06 0.08 249
CF40 a 2.98 0.23 0.13 0.1 458
CF600b 4.12 0.12 0 0.12 127
CF700 b 3.71 0.15 0.06 0.08 249
CF800 b 2.99 0.24 0.12 0.12 475
a
Carbon fibre obtained at different irradiation time (20, 30, 40 min).
b
Carbon fibre obtained at different microwave power (600, 700, 800 W).
c
Barrett-Joyner-Halenda desorption method.
d
Determine at relative pressure p/po ¼ 0.99.
e
Determine by the t-plot method.
f
Obtained by the difference. Mesopore volume ¼ Total pore volume e micropore volume.
g
Brunauer, Emmett and Teller method.

The subsequent microwave pyrolysis had exfoliated the K2O
residues that still remained on the bamboo fibre surface, thus
leaving pores on carbon fibre surface. The use of high microwave
power (800 W) during microwave pyrolysis during the production
of carbon fibre had resulted into more exfoliation of K2O residues
on bamboo surface and leaving more pores on carbon fibre surface.
A high removal of K2O residues is confirmed with zero detection of
K element and a low content of O element detected for CF800
compared to other carbon fibre. Therefore, the use of high micro-
wave power (800 W) during microwave pyrolysis during the pro-
duction of carbon fibre had resulted into more exfoliation of K2O
residues left from KOH treatment and leaving more pores on carbon
fibre. This explained the high total pore volume of CF800 compared
to other carbon fibre.
Fig. 5 shows the SEM micrographs of raw bamboo, bamboo fibre
and carbon fibre obtained from the microwave pyrolysis approach.
Small thread-like fibres were observed in bamboo fibre and all
carbon fibres which can be explained by the removal of protective
lignin bounded to the fibres of bamboo during delignification using
acidified sodium hypochlorite (NaClO2) treatment. Firstly, NaClO2
was dissociated into chlorous acid (HClO2) and sodium ion in an
acidic condition (Eq. (5)). HClO2 was further broken down to form
reactive species such as chlorate ion (ClO 3 ), hypochlorous acid
(HOCl), chlorine dioxide (ClO2) and chloride ion (Cl) (Eq. (6) and
Eq. (7)). During the delignification of bamboo using acidified
NaClO2, cleavage of ether linkages between lignin and hemicellu-
lose lignin had depolymerized lignin through oxidative reaction
by\/*-reactive species of HOCl, ClO2 and ClO 3 . These species were
considered as very strong oxidizing agent that could selectively
break the protective lignin over fibres (Rabetafika et al., 2014; Zhou
et al., 2008). As a result, the breaking down of hemicellulose using
alkaline KOH to produce thread-like structure was easier as the
protective lignin had been removed. The conversion of acidified
NaClO2 treatment into strong oxidizing agent could be summarized
as follows (Ben Sghaier et al., 2012),

Fig. 5. SEM images of raw bamboo (a), bamboo fibre (b) and carbon fibre; CF600 (c), CF700 (d), CF800 (e), CF20 (f), CF30 (g), CF40 (h). The arrows indicate the presence of carbon
nanofibre.
 S.S. Lam et al. / Journal of Cleaner Production 236 (2019) 117692
NaClO2 þ Hþ /HClO2 þ Naþ
2HClO2 / Hþ þ ClO3 þ HOCl
2HClO2 þ HOCl/2ClO2 þ Cl þ H2 O þ Hþ
After microwave pyrolysis of bamboo fibre to form carbon fibre,
the presence of carbon nanofibres (diameter 1 mm) was detected
in CF800 and CF40. This is because of the use of longer irradiation
time (40 min) and higher microwave power (800 W). Generally,
bamboo is made of microfibrils linked by hydrogen bond (Xie et al.,
2016). The longer irradiation time and higher microwave power
could have overcome the strong hydrogen bond between microfi-
bril, thus collapsing the structure of bamboo to produce carbon
fibre in nano size (i.e carbon nanofiber). Therefore, it is worth to
mention that irradiation time and microwave power affect signif-
icantly the diameter size of the carbon fibre obtained.
The capacitive behaviour of carbon fibre was investigated
through cyclic voltammetry (CV). Fig. 6 presents the CV curves of
electrode made from carbon fibre obtained at varying irradiation
time and microwave power of microwave pyrolysis. The CV curve
Fig. 6. CV curves of carbon fibre at scan rate of 5 mV/s over varying microwave power (a) and irradiation time (b).
9
provides information on the capacitive behaviour of carbon fibre
(5) through charge and discharge using three-electrode system. It can
be observed that all CV curves exhibit almost smooth charge and
(6) discharge lines. This can be explained by an electrical double layer
(EDL) occurred at interface between carbon fibre electrode and
(7) KNO3 electrolyte. The EDL was composed of a layer of charges
derived from KNO3 electrolyte ions and a layer of electrical charges
derived from carbon fibre electrode after a potential was applied
through the system.
It can be also observed that there is no presence of significant
redox peak, indicating that non-faradaic reaction was involved
during charging and discharging of carbon fibre (i.e no transfer of
charges). Redox peak is a peak derived from faradaic reaction of
electrode made from metal/transition metal oxides and conductive
polymers (Asen et al., 2018). Thus, the EDL behaviour showed by
carbon fibre electrode suggests that carbon fibre shows potential to
be used in electric double layer capacitor application. The CF800
and CF40 also show better current response compared to others.
This can be explained by their higher surface area that increases the
accessibility of electrolyte ions onto their surface, thus improving
their electrical conductivity (Huang et al., 2014).
10 S.S. Lam et al. / Journal of Cleaner Production 236 (2019) 117692
Table 5
Comparison of carbon fibres produced via microwave pyrolysis and conventional pyrolysis.
Process features Bamboo (this study)
Types of pyrolysis Microwave pyrolysis
Heating source Microwave
Process time 20e40 min
Electrical power (W) 800
Estimated energy consumption (kJ)b 960e1920
Heating rate (
C/min) 30
a
https://www.mtixtl.com/Multi-PositionTubeFurnace-GSL-1100X-NT-UL-1100X-NT-1.aspx.
b
Estimated energy consumption (kJ) ¼ Power of heating source (W)Total process time (s)/1000.
3.4. Comparison of process features with relevant literatures
Table 5 shows the comparison of process features between
microwave and conventional pyrolysis. It can be observed that
carbon fibre produced via microwave pyrolysis offers better process
features as it has shorter process time of 20e40 min and lesser
energy consumption estimated at 960e1920 kJ compared to con-
ventional pyrolysis that consumes longer process time (245 min-8
hours) and more energy consumption (22050e43200 kJ) (Han
et al., 2017; Yang et al., 2018a). Therefore, it is worth to mention
that microwave pyrolysis can provide a potentially economic and
sustainable approach to convert biomass into carbon fibre as it
saves energy and time, thus leading to potential reduction of
manpower, electricity usage and production cost.
4. Conclusions
Carbon fibre was successfully produced from bamboo using a
cleaner approach combining microwave pyrolysis, solvent extrac-
tion, and chemical impregnation. Microwave pyrolysis at high mi-
crowave power (800 W) and high irradiation time (40 min)
produced carbon fibre with high BET surface area (458e475 m2/g),
total pore volume (0.23e0.24 cm3/g) and fixed carbon (78e80 wt
%). The carbon fibre electrode showed positive capacitive behaviour
by storing electrical charges through a mechanism of electrical
double layer. These results demonstrate that microwave pyrolysis
operated under these process conditions is a promising approach to
produce bamboo-based carbon fibre with desirable properties for
use in various applications.
Declarations of interest
None.
Acknowledgements
We acknowledge the financial support of FRGS research grant
(Vot 59434 and 59512) by the Ministry of Education Malaysia and
Golden Goose Research Grant (GGRG) by Universiti Malaysia Ter-
engganu and grateful for the technical and lab support provided by
Henan Agricultural University, Universiti Malaysia Terengganu,
Education University of Hong Kong, Henan University of Technol-
ogy, and Sejong University.
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