j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 3 ( 2 0 0 8 ) 326–332

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

Synthesis and photocatalytic characterization of

titania-supported bamboo charcoals by using sol–gel
method

Chi-Hsin Wu a , Jin-Fang Shr b , Chu-Fu Wu b , Chien-Te Hsieh c,∗

a Institute of Technology Management, Chung-Hua University, Hsinchu 300, Taiwan
b Graduate Institute of Construction Management, Chung-Hua University, Hsinchu 300, Taiwan
c Department of Chemical Engineering and Materials Science, Fuel Center, Yuan Ze University, Taoyuan 320, Taiwan

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

Article history: The present work examined the photocatalytic behavior of methylene blue (MB) on titania-
Received 18 July 2007 dispersed bamboo charcoals, prepared by sol–gel method combined with chemical-wet
Accepted 13 October 2007 impregnation. The experimental results of nitrogen adsorption showed that specific sur-
face area of the TiO2 -charcoals was found to increase with TiO2 loading, whereas their mean
pore sizes exhibited a decreasing trend. It can be suggested that TiO2 nanoparticles were
Keywords: mostly coated on the charcoal surface and partially deposited in the mouth of pore chan-
Titania nels. Our preparation technique for the heterogeneous catalysts improves the dispersed
Bamboo charcoals degree of TiO2 catalyst, which shows a better photocatalytic performance than pure TiO2
Photocatalysis aggregation. A linearity relationship between the overall photocatalytic efficiency and the
Elovich kinetic model TiO2 loading reflected that each titania particle behaves an identical photocatalytic reac-
Methylene blue tivity. The liquid-phase photocatalytic behavior of the heterogeneous catalysts can be well
described by Elovich kinetic model.
© 2008 Published by Elsevier B.V.

1. Introduction liquid-phase photodegradation mechanism, it is generally rec-

Titanium dioxide (or called titania) is a particularly versatile
material with technological applications, such as photo-
catalyst, photovoltaic material, gas sensor, optical coating,
dye-sensitized cell, structural ceramic, and more (Mor et al.,
2005). Among these applications, anatase-type TiO2 photocat-
alyst has attracted a great deal of interests due to its redox
capability under ultraviolet (UV) irradiation, i.e., usually the
wavelength <385 nm. This unique character leads to exten-
sive use in degradation of organic compounds, deodorization,
and anti-bacterial treatment (Ohko et al., 2001; Harada et al.,
2002; Sehili et al., 1989; Villasenor et al., 1998; Driessen et al.,
1998; Anpo and Takeuchi, 2003; Asahi et al., 2001). Probing to
ognized that conduction band electrons (e− ) and valence band
holes (h+ ) are first generated on the surface of photocatalyst
particles when the aqueous catalyst suspension is illuminated
by light with an energy greater than the band gap energy, i.e.,
3.2 eV (Lin et al., 2005; Guo et al., 2006). The adsorbed pollu-
tant molecules onto the nanocatalysts are then oxidized by
free radicals, e.g., hydroxyl radicals (• OH) formed in aqueous
solution (Yu et al., 2005a,b; Ge and Xu, 2006), thereby resulting
in the photocatalytic effect.
There have been significant efforts to develop different
forms of nanocatalysts, including high-voltage acceleration
technique (Anpo, 2000), sol–gel method (Dvoranová et al.,
2002), coprecipitation–peptization (Li et al., 2005), DC plasma

∗
Corresponding author. Tel.: +886 3 4638800x2577; fax: +886 3 4559373.
E-mail address: cthsieh@staurn.yzu.edu.tw (C.-T. Hsieh).
0924-0136/$ – see front matter © 2008 Published by Elsevier B.V.
doi:10.1016/j.jmatprotec.2007.10.073
 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 3 ( 2 0 0 8 ) 326–332
(Lin et al., 2005), and template-assisted synthesis (Mor et al.,
2005). These abilities to fabricate various nanoarchitectures
are expected to positively impact realistic applicability. Up
to now, the improvement of the photocatalytic reactivity still
seeks for further investigations. One way to improve the pho-
tocatalytic capability is to increase available active areas for
photodegradation of pollutant molecules in vapor- or liquid-
phase. Indeed, the selection of a suitable support as host
material is necessary for the above purpose. There are several
porous media, such as zeolite, carbon nanotube, aerogel, and
active carbon, which as far as possible provide pore structures
for dispersing TiO2 photocatalysts. Pioneer researchers have
prepared TiO2 -coated or -mounted composites, which show
the improvement of photocatalytic efficiency or kinetic, com-
paring to the raw titania catalyst (Zou et al., 2006; Robert et
al., 1999; Tryba et al., 2003; Matos et al., 1998, 2001). Apart
from the supports mentioned above, bamboo charcoal is an
emerging material due to its multi-functionality, including
high mechanical strength carbon composite (Qiao et al., 2002),
and adsorbents in removing odor and volatile organic com-
pounds (VOCs) (Abe et al., 2001; Mizuta et al., 2004). In general,
such natural carbon possesses a regular and parallel pore-
channels infrastructure, i.e., lengthwise and crosswise, which
came from the original lignocellulose of bamboo (Qiao et al.,
2002; Abe et al., 2001; Mizuta et al., 2004). These well-ordered
nanochannels are credited to be an excellent catalyst sup-
port, which may facilitate less adsorption resistance. This
probably promotes the photocatalytic kinetic of the pollutant
molecules.
The present work aims to provide an efficient TiO2 -coated
bamboo charcoal in degrading methylene blue (MB, molecu-
lar formulation: C16 H18 ClN3 S; MW: 320) in liquid phase. This
organic compound is one of the common contaminants in
wastewater, and many efforts have been made in removing MB
by using adsorption technique (Lin and Teng, 2002). Removal
of MB via the photocatalysis probably is a promising way due
to its simplicity, low cost, and convenience (without follow-up
treatments). Here we prepared three surface loadings of TiO2
nanoparticles onto bamboo charcoal by sol–gel, followed by
chemical-wet impregnation. In the present work, we propose a
kinetic model, Elovich equation, to examine the photocatalytic
behavior.
2. Experimental procedure
In the present work, the bamboo charcoal powder was sup-
plied from Industrial Technology Research Institute, Taiwan.
According to its specification, this type of charcoal was pre-
pared through a carbonization treatment at 700 ◦ C. Prior to
surface modification, the charcoals were grinded and then
sieved into a desired particle size of 10–40 ␮m. A chemical oxi-
dation treatment was carried out to implant surface oxides
onto the carbon surface. The charcoal powders were impreg-
nated with nitric acid solution (0.1N), and then the carbon
slurry was well stirred via a magnetic bar at 90 ◦ C for 6 h.
This chemical-oxidation treatment enables to implant oxide
groups on the dangling bond of carbon, thus leaving hydroxyl
and carboxyl groups. These implanted oxides would promote
surface polarity or hydrophilicity due to the improvement of
327
electrostatic force (Kinoshita, 1987; Toebes et al., 2004; Hsieh
and Teng, 2002), which is expected to reinforce the interface
affinity between TiO2 nanoparticles and the oxidized bamboo
charcoal.
A Ti-containing polymeric sol was prepared by mixing tita-
nium isopropoxide Ti(OC3 H7 )4 (reagent grade, Aldrich) and
ethanol/D.I. water (1:1 in v/v). Hydrochloric acid (0.1N) was
used to adjust the pH value of the Ti-containing sol (pH
2). To investigate the influence of TiO2 loading on photo-
catalytic activity, we prepared three molar concentrations of
Ti-containing sols (0.2, 0.4, and 0.6 M). The transparent sols
were magnetically stirred at room temperature for 8 h. After
that, the oxidized charcoal samples (3 g) were impregnated
in the resulting Ti sols (30 mL) at 30 ◦ C, i.e., at the fixed vol-
umetric ratio of solid to liquid (1:10). This wet-impregnation
process was carried out at ambient temperature for a period
of 2 h, making the dispersion of titania nanoparticles onto the
surface of bamboo charcoal. Finally, the carbon slurries were
heated from room temperature to 400 ◦ C with a linear heating
rate of 10 ◦ C min−1 , and held at this temperature for 0.5 h. The
heat treatment was progressed in tubular furnace, in which
stainless-steel tube (inner diameter: 5 cm; length: 80 cm) was
inset inside, under a nitrogen atmosphere with the steady flow
rate of 300 mL min−1 .
Field emission-scanning electron microscope (FE-SEM,
LEO 1530) was used for morphological observations of the
TiO2 -coated charcoals. Surface characteristics of TiO2 -loaded
bamboo charcoals, such as specific surface area and poros-
ity, were determined by N2 adsorption at −196 ◦ C, using an
automated adsorption apparatus (Micromeritics ASAP 2000).
MB photodegradation tests were carried out to examine the
photocatalytic capability of TiO2 -loaded bamboo charcoals.
The photodegradation of MB solutions was characterized by
an UV–vis spectrometer (Shimazu UV-2550). The MB wave-
length prevailingly absorbed by formaldehyde is concentrated
at 664 nm. Based on the Beer–Lambert law, the concentra-
tion of phenol aqueous solution is linearly proportional to
the absorbance of measured spectrum in the concentration
range around 500 mg L−1 . In the present study, the MB solution
(100 mL) containing 0.2 wt.% of well-dispersed titania-coated
charcoal nanoparticles was illuminated by employing a 13 W
fluorescent lamp, which has an incident intensity of illumina-
tion of 750 ␮W cm−2 .
3. Results and discussion
3.1. Surface characteristics of the resulting
heterogeneous catalysts
The as-synthesized titania nanospheres onto bamboo char-
coals are designated as TiC followed by weight percentage of
TiO2 loading to charcoal, i.e., TiC5, TiC10, and TiC15. Fig. 1(a)
and (b) shows FE-SEM images of TiO2 -charcoal composites
(TiC15) with low- and high-magnifications, respectively. It can
be seen that the TiO2 particulates are uniformly dispersed
over the charcoals, and no obvious aggregation of titania par-
ticle was found. The diameter of titania sphere is essentially
the same (20–40 nm) for the TiO2 coating on charcoal surface.
This result can be explained within the context of the forma-
328 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 3 ( 2 0 0 8 ) 326–332
Fig. 1 – Typical FE-SEM photographs with (a) low- and (b)
high-magnification for bamboo charcoal attached with
titania nanoparticles prepared by the chemical-wet
impregnation technique.
tion mechanism of titania-coated charcoals. The pre-chemical
oxidation by nitric acid may create oxide groups, which were
uniformly grown on the surface and in the vertical pore of
charcoal. During the wet impregnation, each oxide group acts
as an active site in adsorbing Ti4+ ions in liquid phase. This
interaction would favor to take place on the oxides until the
equilibrium state is reached. At higher TiO2 sol concentration,
more oxide group sites would be occupied, thus forming a
higher coverage of Ti–O containing intermediate on the oxi-
dized charcoal surface.
N2 physisorption at −196 ◦ C was used to determine sur-
face characteristics of the TiO2 -coated charcoals. Typical
N2 isotherms of the prepared charcoals are represented in
Fig. 2(a). These isotherms are of Type II, indicating that these
carbon samples are mainly mesoporous. It is also found
that these isotherms have different shapes within relative
pressure region between 0.5 and 0.8, implying various meso-
pore size distributions in the charcoals. According to N2
adsorption isotherms, surface characteristics of the charcoal
samples, including specific surface area, total pore volume,
and pore size distribution, can be determined and are col-
Fig. 2 – (a) Adsorption isotherms of nitrogen onto
titania-loaded charcoals at −196 ◦ C. (b) Pore size
distributions of titania-loaded charcoals determined by BJH
technique.
lected in Table 1. In comparison, the original charcoal was also
employed as a reference. As shown in Table 1, the specific sur-
face areas of the charcoal samples show an obvious increase in
comparing to the starting material, which has a surface area
of ca. 30.5 m2 g−1 . This enhancement of surface area can be
inferred that titania nanoparticles coated on carbon surface
provide surface area for N2 adsorption. In addition, the TiO2 -
attached charcoals have mainly mesoporosity, i.e., >87.5% in
mesopore fraction. This finding demonstrates that after TiO2
coating, the bamboo charcoal still maintains a well-developed
pore structure.
It is of interest that the specific areas are not proportional to
the pore volumes, reflecting different mesopore size distribu-
tions in these samples. Barret–Joyner–Halenda (BJH) method
was employed to analyze the mesopore size distribution, and
the results are shown in Fig. 2(b). All distributions are relatively
 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 3 ( 2 0 0 8 ) 326–332 329

Table 1 – Surface characteristics of titania-coated bamboo charcoals determined by nitrogen physisorption at −196 ◦ C
Sample type SBET a (m2 g−1 ) Vt b (cm3 g−1 ) Pore size distribution Peak pore

Vmicro d (%) Vmeso e (%) size, Df (Å)

Charcoal 30.5 0.030 2.0 98.0 78.5

TiC5 35.3 0.036 5.6 94.6 69.1
TiC10 49.8 0.052 8.9 91.1 49.2
TiC15 66.7 0.072 12.5 87.5 38.8

a
Specific surface area computed using BET equation.
b
Total pore volume estimated at a relative pressure of 0.98.
d
Micropore volume determined from the Dubinin–Radushkevish equation.
e
Mesopore volume determined from the subtraction of micropore volume from total pore volume.
f
Peak pore size from the pore size distribution determined by Barrett–Joyner–Halenda (BJH) method.

narrow, ranging between 20 and 100 nm. It is obvious that the

peak position in the distributions has a decreasing trend with
increasing titania loading. The maximum in the distributions
has following order: TiC5 (6.91 nm) > TiC10 (4.92 nm) > TiC15
(3.88 nm), which is also listed in Table 1. This result is pre-
sumably due to that the attachment of TiO2 nanoparticles not
only takes place on the surface of charcoal, but also partially
blocks the pore channels. This transformation in mesopore
size distribution may be a crucial factor in determining the
photocatalytic kinetic of MB in aqueous solution.
Fig. 3 depicts the XRD patterns of the titania–charcoal sam-
ples calcined at the heat-treated temperature of 400 ◦ C. Here
a board peak concentrated at ca. 26◦ can be attributed to two
types of crystalline structures. The first peak is the anatase
[1 0 1] diffraction at a scattering angle (2) of 25.3◦ (Tsai and
Teng, 2004). The other broad peak at 26.2◦ corresponds to
the existence of amorphous carbon from the charcoal. As
observed in Fig. 3, the peak intensity of other indicated anatase
peaks are almost proportional to TiO2 loading. This result

Fig. 4 – Liquid-phase photodegradation kinetics of MB on

the titania-loaded charcoals at 30 ◦ C.

reflects that all titania onto charcoals has the same crystalline
structure even at low- and high-surface loadings.

3.2. Photodegradation of MB on the heterogeneous

catalysts

Fig. 4 shows the photodegradation efficiency of MB as a

Fig. 3 – XRD patterns for charcoals attached with different
loadings of titania nanoparticles prepared by the
chemical-wet impregnation technique.
function of irradiation time for all titania-coated bamboo
charcoals under an UV ray ( < 400 nm). For all charcoals, the
removal efficiency of MB rapidly decreases, and then gradu-
ally decays after the first 1 h. It is expected that TiO2 -dispersed
shows a photocatalytic capability better than raw TiO2 powder.
Moreover, the overall removal efficiency of the TiO2 -attached
charcoal increases with TiO2 loading. The above results can
be attributed to a fact that (1) well-dispersed TiO2 onto char-
coal would behave a greater photocatalytic activity than TiO2
aggregation in liquid phase; (2) higher titania surface cover-
age leads to generate a greater amount of electron/hole pairs,
capable of degrading MB molecules in liquid phase, thus pro-
moting the effectiveness of photocatalysis.
330 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 3 ( 2 0 0 8 ) 326–332

Table 2 – The most suitable Elovich parameters for

photodegradation of MB by using titania-coated bamboo
charcoals under UV Irradiation
Sample ˛ (mg g−1 min−1 ) ˇ (g mg−1 ) t0 (min) r2
type

TiC5 0.125 0.87 9.20 0.990

TiC10 0.149 2.27 2.96 0.987
TiC15 0.152 4.99 1.32 0.985

Yu et al., 2005b). Even if the bamboo charcoal likely perturbs

the transmission of UV light to the surface of titania; however,
our preparation enables to coat the TiO2 particulates mostly
onto the surface of charcoal and partially in the mouth of pore
channels, as shown in Fig. 1. This proves that the above consid-
eration seems so minor, and the titania catalysts can directly
be excited by UV transmission. In addition, it significantly
compensates the above inhibition by a strong beneficial effect
in MB adsorption followed by a mass transfer of MB to TiO2
Fig. 5 – Variations of removal efficiency and Elovich
particles. Therefore, the existence of charcoal can be served
parameter (˛) with titania loading.
as two important roles for catalyst support and transport of
MB, leading to the enhancement of photocatalytic capability.

It can be found that the photocatalytic efficiency adheres

to linear increase with TiO2 loading, as illustrated in Fig. 5.
This linearity relationship reflects that each titania particulate
behaves an identical photocatalytic reactivity. Our prepara-
tion technique for the heterogeneous catalysts improves the
dispersed degree of TiO2 catalyst, which shows a better pho-
tocatalytic performance than pure TiO2 aggregation.
A possible MB photocatalytic mechanism on TiO2 -loaded
charcoal in liquid phase can be proposed as following three
steps. At the first step, it is reasonable to suggest that liquid-
phase adsorption of MB initially occurs on pore structure of
charcoal. Secondly, TiO2 particulates on charcoal can adsorb
UV light with an energy greater than 3.2 eV to generate elec-
tron/hole pairs, as shown in Eq. (1). The hole (h+ ) are ultimately
trapped with OH− ions or with H2 Oads on the TiO2 particulate
surface to yield H+ and hydroxyl radicals (OH• ), as shown in
Eq. (2). Concomitantly, oxygen molecules react with conduc-
tion band electron (e− ) to produce superoxide radical anion
(O2 •− ), and then generates the hydroperoxide radical OOH•
(Eq. (3)) (Kaneco et al., 2006).
 
hv>3.2 eV e−
TiO2 −→ TiO2 → e− + h+
h+
h+ + OH− (or H2 O)surf → OH• (+H+ )
− +
e + O2 → O2 •− + H → OOH•
3.3. Analysis on photocatalytic kinetic by Elovich rate
equation
To numerically examine the photocatalytic activity, a conven-
tional mechanism, Langmuir–Hinshelwood (LH) model, with
the rate being proportional to adsorptive surface coverage has
been extensively employed in pervious studies (Zou et al.,
2006; Matos et al., 1998, 2001; Kaneco et al., 2006). However,
this simple model cannot give a fairly good simulation to our
heterogeneous photocatalyst in degrading MB molecules from
liquid phase. For this purpose, an empirical kinetic model,
Elovich rate equation, is applied here and given as follows
(Önal, 2006; Chang et al., 2004; Teng and Hsieh, 1999):
dqt
r= = ˛ exp[−ˇqt ] (1)
dt
where r (or dqt /dt) is the photocatalytic rate in unit of
mg g−1 min−1 , ˛ is the initial rate mg g−1 min−1 when qt
approaches zero (i.e., at irradiation time t = 0), and ˇ is related
to the extent of surface coverage for photocatalytic activity of
MB degradation. Integrating Eq. (1) with the condition (qt = 0
(1)
at t = 0) and subsequently linearizing the integrated equation
results in
(2)
1 1
qt = ln(t0 ) + ln(t + t0 ) (2)
ˇ ˇ
(3)

where t0 is equal to 1/˛ˇ. If ˛ˇt  1, Eq. (2) can further be sim-

OH• (or OOH• ) + MB → → oxidative products (4)
plified as

As shown in Eqs. (1)–(3) the strong oxidants associated 1 1

with hydroxyl radicals react with the MB, thus degrading MB qt = ln(˛ˇ) + ln(t) (3)
ˇ ˇ
molecules into oxidative products. Since decomposition reac-
tion of MB molecules is composed of several steps, Eq. (4) is A plot of qt versus ln t can give the apparent Elovich rate
just a simplified form. constants, ˛ and ˇ, from the intercept and the slope of the
In the third step, once the dye occupied on the active site linearity equation. The values of Elovich parameters, together
is degraded, another dye molecule would enter and occupied with correlation factors (r2 ), for all TiO2 -attached charcoals are
on this site through a diffusion phenomenon (Lin et al., 2005; collected in Table 2.
 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 3 ( 2 0 0 8 ) 326–332
According to the above results, an increasing ˛ value is gen-
erally accomplished with increasing TiO2 loading, as depicted
in Fig. 5. However, it is worth to note that this initial pho-
tocatalytic rate is not proportional to TiO2 surface coverage.
This finding can be attributed to a fact that the MB transport
cannot easily penetrate into the pore structures, which was
partially blocked at high-titania coverage. This can be demon-
strated by analysis of mesopore size distribution, as shown in
Fig. 2(b). Therefore, charcoal nanochannels with larger pore
size would facilitate a greater photocatalytic kinetic for MB
degradation due to less pore diffusion resistance. Additionally,
the most suitable Elovich parameters in Table 2 are used to pre-
dict the photodegradation kinetics of MB in aqueous solution
with different TiO2 -loaded charcoals. The simulation curves
of removal efficiency versus irradiation time are presented in
Fig. 4 to compare with the experimental data. We observe that
the Elovich model provides an equally good fit for all samples
within the entire irradiation time. This satisfactory result of
the present work demonstrates that the photocatalytic kinetic
of the heterogeneous photocatalyst can be well described by
the Elovich model.
4. Conclusions
Titania-dispersed bamboo charcoals were prepared to inves-
tigate their photocatalysis of methylene blue (MB) in liquid
phase. A sol–gel combined with chemical-wet impregnation
enabled to well disperse TiO2 particulates onto the per-
oxidized charcoals. Specific surface area of the TiO2 -charcoals
was found to increase with TiO2 loading, whereas their mean
pore sizes showed a decreasing trend. It can be suggested that
TiO2 particulates were mostly coated on the charcoal surface
and partially into the mouth of pore channels. Liquid-phase
photocatalysis of MB showed that the TiO2 -loaded charcoals
exhibit a better photodegradation efficiency, comparing with
pure TiO2 aggregation. It was also found that the overall pho-
tocatalytic efficiency is proportional to TiO2 surface coverage,
and the initial photocatalytic rate is affected by the meso-
pore size distribution of charcoals according to the analysis
of Elovich kinetic model. These findings demonstrated that
the existence of charcoal acts as a critical role for improving
catalyst dispersion and transport of MB.
Acknowledgment
The authors gratefully acknowledge the financial support
from the National Science Council (NSC) of Taiwan, through
Project No. NSC 95-2221-E-155-079.
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