December 2002

Materials Letters 57 (2002) 818 821

www.elsevier.com/locate/matlet

Rice husk ash as an alternate source for active silica production

V.P. Della a,*, I. Kuhn a,b, D. Hotza a,c
a

Graduation Program in Materials Science and Engineering (PGMAT), Federal University of Santa Catarina (UFSC),
P.O. Box 476, 88040-900 Florianopolis, SC, Brazil
b
Department of Mechanical Engineering (EMC), Federal University of Santa Catarina (UFSC), P.O. Box 476,
88040-900 Florianopolis, SC, Brazil
c
Department of Chemical Engineering (EQA), Federal University of Santa Catarina (UFSC), P.O. Box 476,
88040-900 Florianopolis, SC, Brazil
Received 18 September 2001; received in revised form 23 April 2002; accepted 23 April 2002

Abstract
The objective of the present work is to develop a procedure for obtaining and characterization active silica with a high
specific surface area from rice husk ash. The relative amount of silica was increased after burning out the carbonaceous material
at different times and temperatures. A 95% silica powder could be produced after heat-treating at 700 jC for 6 h. The specific
surface area of particles was increased after wet milling from 54 to 81 m2/g.
D 2002 Elsevier Science B.V. All rights reserved.
Keywords: Rice husk; Rice husk ash; Active silica; Specific surface area

1. Introduction
The beneficiation of rice generates as by-product
rice husk that corresponds to about 23% of its initial
weight. This husk can be used as a fertilizer in
agriculture [1] or as an additive for cement and
concrete fabrication [2,3]. Due to its high silicon
content, rice husk has become a source for preparation
of elementary silicon [4,5] and a number of silicon
compounds [6], especially silica [7,8], silicon carbide
[9,10] and silicon nitride [10].
Many authors [4,7,11 15] have concluded that
preliminary leaching of rice husks with a solution of

Corresponding author. Tel.: +55-48-3319268; fax: +55-482340059.

E-mail address: viviana@pg.materiais.ufsc.br (V.P. Della).

HCl, HNO3, H2SO4, NaOH and NH4OH, boiled

before thermal treatment with temperatures ranging
from 500 to 1400 jC for various time intervals
[16,17], proved to be effective in substantially removing most of the metallic impurities and producing ashsilica completely white in colour with a high specific
surface area.
An increasing application of rice husk is as fuel in
heat generation for drying rice, due to its high
calorific power (approximately 16720 kJ/kg). In this
combustion, rice husk ash (RHA) is produced. The
burning of rice husk in air always leads to the
formation of silica ash, which varies from gray to
black depending on inorganic impurities and unburned carbon amounts [18].
In this paper, processing and characterization of
high specific surface area silica from RHA is presented. The relative amount of silica was increased by

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V.P. Della et al. / Materials Letters 57 (2002) 818821

Table 1
Chemical composition of RHA before and after burning out at 700
jC for 6 h
Components expressed
as oxides

RHA
as received

RHA after
burning out

SiO2
Al2O3
Fe2O3
CaO
Na2O
K2O
MnO
TiO2
MgO
P2O5
Loss on fire

72.1
0.30
0.15
0.43
0.50
0.72
0.15
0.05
0.70
0.06
24.3

94.95
0.39
0.26
0.54
0.25
0.94
0.16
0.02
0.90
0.74
0.85

heat treatment and the specific surface area was

improved by milling.

2. Experimental procedure
The raw material used for the experiments was an
RHA obtained from a local Industry (Fumacense,
Morro da Fumaca, SC, Brazil) after burning rice husk
during the process of rice manufacture.
The first step for producing a high specific surface
area silica or active silica (AS) from RHA consists of
a thermal treatment at several temperatures. The aim
of this step is to increase the relative amount of
silicon oxide by reduction of carbonaceous materials
present in the samples, as well as to burn out other
undesirable components detected by chemical analysis. The ash samples were submitted to heat treatment
in ceramic crucibles of 24.5 cm diameter (Oxford,
Sao Bento do Sul, SC). Heating cycles were carried
out in air in an electric oven (Shaly, model Lab 181300CR) with a heating rate of 10 jC/min. Each
sample was held at a maximum temperature (400,
500, 600 or 700 jC) for 1, 3 or 6 h. The samples were
cooled down inside the oven.
The grinding step to decrease mean particles size
and increase specific surface area was carried out in a
high impact mill (Gabrielli, model Mill2) with a
porcelain jar and microspheres of high alumina as
grinding medium. Wet milling cycles of 10, 40 and 80
min were performed.
Quantitative chemical analyses of RHA were
accomplished by X-ray fluorescence (XRF, Philips,

819

model PW 2400, The Netherlands). Mineralogical

analysis was performed by X-ray diffractometry
(XRD, Philips, model Xpert, The Netherlands) with
CuKa radiation. The of particles size distribution was
determined by laser diffraction (Cilas, model 1064L,
USA). Specific surface area of RHA particles was
determined by the nitrogen adsorption according to
B.E.T. (Micrometrics, model ASAP 2000, USA). The
carbon analysis was performed according to ASTM
5373 [19] by IR spectroscopy (Leco, model CHN
600, USA).

3. Results and discussions

The RHA sample after burning out at 700 jC for 6
h presented the highest amount of silica (Table 1)
compared to the other samples. This sample was
chosen to be submitted to grinding. The relative
contents of other elements increased in general with
increase in temperature and time [14]. Small divergences of this rule are probably caused by inherent

Fig. 1. XRD of RHA: (a) as received; (b) after burning out at 700
jC for 6 h.

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V.P. Della et al. / Materials Letters 57 (2002) 818821

noticed, indicating an incipient crystallization process

leading to a disordered cristobalite [21].
Patel [14] reported that the temperature of carbonization is preferably below 700 jC to avoid any transformation of amorphous to crystalline form. It has been
found that reheating the ash to remove carbon residues
takes a relatively long period of time and higher
temperatures, with the consequent effect that silica is
converted to crystalline forms [22]. This behavior was
not evidenced along the burning cycles here applied.
The structure of silica present in the ash treated at 700
jC for 6 h remained essentially amorphous (Fig. 1b).
It has been found that reheating the ash to remove
carbon residues takes a relatively long period of time
and higher temperatures, with the consequent effect
that silica is converted to crystalline forms [22]. This
behavior was not evidenced along the burning cycles
here applied.

Fig. 2. Particle size distribution of RHA: (a) as received; (b) after

wet grinding for 80 min in a jar mill.

uncertainty of measurements. The percentage of loss

on fire decreased after heat treatment. The most
common trace elements in RHA are sodium, potassium, calcium, magnesium, iron, copper, manganese
and zinc [20]. Differences in composition are due to
geographical factors, year of harvest, sample preparation and analysis methods.
Burning out temperature and time are important
factors to define whether silica remains amorphous, as
in RHA, or become crystalline. In spite of higher
temperatures and times of heat-treating applied in this
study, the structure of silica present in the ash remained
essentially amorphous (Fig. 1a). For the samples RHA
400 jC for 6 h, 500 jC for 1 h, 500 jC for 3 h and 500
jC for 6 h, a diffused peak at about h = 22j was

Fig. 3. Macroscopies of RHA: (a) as received; (b) after burning out

at 700 jC for 6 h, and wet grinding for 80 min in a jar mill.

V.P. Della et al. / Materials Letters 57 (2002) 818821

The particle mean size of RHA after burning out at

700 jC for 6 h was around 33 Am (Fig. 2a), being all
particles lower than 112 Am. After milling for 80 min,
the mean size was decreased to 0.68 Am, being 100%
of particles lower than 6 Am (Fig. 2b).
As raw material, RHA presented a specific surface
area around 177 m2/g. After burning out at 700 jC for
6 h, it was changed to 54 m2/g. This decrease in
specific area is proportional to heating temperature
and time, which causes an agglomeration effect,
diminishing porosity. After wet grinding for 80 min,
the particles specific area increased to 81 m2/g.
The carbon content was estimated as the percent loss
on fire [7]. Color changes are associated with the
completeness of combustion process as well as with
structural transformation of the silica in the ash. Houston [20] has classified RHA into high-carbon char, lowcarbon gray ash, and carbon-free pink or white ash.
The as-received RHA samples are black with some
gray particles, resulting from different stages of the
carbon combustion during burning of rice husk (Fig.
3a). The active silica obtained after the heating and
grinding presents reduced size of particles and gray
coloration due to the lower content carbonaceous
material (Fig. 3b). The level of carbon detected in
RHA before thermal treatment was 18.60%. The level
of carbon decreased considerably after the thermal
treatment, being of 0.14% for the RHA 700 jC for 6 h
sample (Fig. 3b).
The amount of black particles decreased with
increase in calcination temperature and time. At
700 jC for 6 h, the thermal treatment yielded bright
white silica.

4. Conclusions

It was possible to obtain high specific area silica

from the rice husk ash after heat-treating and
milling processing by applying this simple technique, and it is possible to transform industrial
residue in useful raw materials, avoiding damage to
the environment.

Acknowledgements
The financial support of the Brazilian Agency
CAPES is acknowledged.

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Within the limits of the present studies, the following conclusions can be drawn:
Rice husk ash is an alternative source for high
specific area silica.
A 95% silica powder could be produced after
calcination at 700 jC for 6 h. The specific surface
area of particles was increased after wet milling
from 54 to 81 m2/g.
The thermal treatment of rice husk ash does not
affect the structure of its ash-silica.

821

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