Journal of Experimental Nanoscience

ISSN: 1745-8080 (Print) 1745-8099 (Online) Journal homepage: https://www.tandfonline.com/loi/tjen20

High-purity nano silica powder from rice husk

using a simple chemical method

R. Yuvakkumar , V. Elango , V. Rajendran & N. Kannan

To cite this article: R. Yuvakkumar , V. Elango , V. Rajendran & N. Kannan (2014) High-purity
nano silica powder from rice husk using a simple chemical method, Journal of Experimental
Nanoscience, 9:3, 272-281, DOI: 10.1080/17458080.2012.656709

To link to this article: https://doi.org/10.1080/17458080.2012.656709

Published online: 04 Jul 2012.

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Journal of Experimental Nanoscience, 2014
Vol. 9, No. 3, 272–281, http://dx.doi.org/10.1080/17458080.2012.656709

High-purity nano silica powder from rice husk using a simple chemical method
R. Yuvakkumara, V. Elangoa, V. Rajendrana* and N. Kannanb
a
Centre for Nanoscience and Technology, K.S. Rangasamy College of Technology, Tiruchengode 637215,
Tamil Nadu, India; bDepartment of Biotechnology, K.S. Rangasamy College of Technology, Tiruchengode
637215, Tamil Nadu, India
(Received 28 July 2010; final version received 8 January 2012)

A highly pure, small particle-sized and high surface area nano silica powder was prepared from
rice husk using alkali extraction, followed by an acid precipitation method. The composition,
phase, morphology, size and surface area of the as-synthesised nano silica powder was
investigated by energy-dispersive spectroscopy, Fourier transform infrared spectroscopy, X-ray
diffraction, transmission electron microscopy, particle size analyser and BET surface area
analyser. High-purity nano silica powder was obtained by sodium hydroxide (NaOH)
purification treatment (0.5, 1, 1.5, 2 and 2.5 N). The high purity of silica (99.9%) was obtained
at 2.5 N NaOH treatment. The pure nano silica powder that is obtained shows an average particle
size of 25 nm with a high-specific surface area (SSA) of 274 m2 g1, with an average pore
diameter of 1.46 nm.
Keywords: high purity; nano silica; rice husk; surface area

1. Introduction
Nano silica powder is widely used in areas such as ceramics, chemicals, catalysis, chromatog-
raphy, energy, electronics, coatings, stabilisers, emulsifiers and biological sciences [1–5]. In view
of large-scale industrial applications, an enormous quantity of nano silica powder with
controlled shape, size and porosity is required [6,7]. The nano silica powder is generally prepared
by using vapour-phase reaction, sol–gel and thermo-decomposition [8–12] methods. In most of
the above-mentioned methods, nano silica powder is synthesised using chemicals as a raw
material. In chemical methods, it is easy to control size, shape and purity of the material but the
starting reagents are costly. In industrial applications, low costs and large quantities of initial
precursor are needed. Rice husk is one of the most abundant by-products produced in the paddy
field. The agricultural by-product includes rice husk, rice straw, plant materials and so on. Of all
these by-products, rice husk contains more than 95% silica. Hence, several attempts have been
made to produce bulk silica from the most eco-friendly and economical source rice husk [13–18].
The review confirms that rice husk is an excellent source for the production of high-grade
amorphous bulk silica powder. In recent years attempts have been made to prepare nano silica
powder from rice husk [19–24].
To the best of our knowledge, very few attempts have been made to prepare high-purity
nano silica powder from rice husk ash (RHA). The amorphous nanostructured silica
powder with an average particle size of 60 nm and a SSA of 235 m2 g1 has been obtained by

*Corresponding author. Email: veerajendran@gmail.com

ß 2012 Taylor & Francis

 Journal of Experimental Nanoscience 273

non-isothermal decomposition of rice husk in an oxidising atmosphere [19]. Zaky et al. [20]
prepared nano silica particles from semi-burned rice straw ash by a two-step procedure of
electro-deposition and reduction, and investigated their electronic and mechanical properties.
Real et al. [21] synthesised homogeneous nano-sized silica particles by burning rice husk at
1073 K in a pure oxygen atmosphere. Conradt et al. [22] have investigated the potential and
limits of using rice husk as a competitive source of nano-structured silica. The size distribution
of secondary particles (agglomerates of two or three primary nano particles) was about 26 nm
and the SSA of the primary particles was 250 m2 g1. Therefore, it is of great interest and
significance to investigate the development of highly pure nano silica powder from naturally
available raw material, i.e. rice husk, at low cost with high efficiency.
In the present investigation, an attempt has been made to produce highly pure, small
particle-size nano silica powder with high-surface area from agricultural by-product, such as rice
husk, by using a simple user-friendly, alkali extraction followed by an acid precipitation method.
The method is simple, cost-effective, reliable and reproducible. The main difference between
work carried out by the conventional method [19–22] and the work reported in this study is the
effect of different concentrations of sodium hydroxide (NaOH) on high-purity nano silica
powder. The optimum conditions to achieve high-purity nano silica have been studied. In
addition, the synthesis of nano silica powder is carried out by muffle furnace without oxygen
environment. In conventional methods, nano silica particles are prepared under oxygen
atmosphere. The purity obtained by this method is enhanced to currently available conventional
methods. Further, the nano silica powder that is prepared, has been comprehensively tested
using energy-dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR),
X-ray diffraction (XRD), transmission electron microscopy (TEM), particle size analyser (PSA)
and BET surface area analyser to explore the structure, morphology, size and other properties.

2. Experimental
2.1. Synthesis of high-purity nano silica powder
The pure nano silica powder was extracted from RHA by controlling different process
parameters. The raw material, rice husk, was obtained from a rice mill and washed thoroughly
with distilled water to remove any adhering impurities. The washed rice husk was air-dried at
room temperature and then burnt at 973 K for 3 h in a muffle furnace under an inert
atmosphere. The obtained RHA was washed with distilled water to neutralise the pH in order to
remove the sand, dust, light empty grains and fine dirt. Hence, the repeated washing of RHA
neutralises the pH and removes the adhered impurities on the surface of silica. The neutralised
RHA was refluxed with 6 N HCl (Merck GR) for 1.5 h and then filtered in order to remove
metallic impurities and to extract pure nano silica. The filtered RHA was thoroughly rinsed with
hot water repeatedly and then boiled with different concentration of NaOH (Merck GR)
solutions at 353 K for 1.5 h, while being stirred magnetically, and was then filtered to obtain
sodium silicates, after the reaction,
SiO2 ðashÞ þ NaOH ! Na2 SiO3 þ H2 O ð1Þ
The obtained residue was thoroughly washed with hot water for complete extraction of
sodium silicate. The obtained pH of the filtrate (sodium silicate) was reduced to 2.0 using
controlled addition of concentrated H2SO4, while being stirred magnetically, to extract the nano
silica precipitates. The chemical reaction that takes place during the above process is
Na2 SiO3 þ H2 SO4 ! SiO2 þ Na2 SO4 þ H2 O ð2Þ
274 R. Yuvakkumar et al.

The obtained precipitate was washed thrice in warm distilled water and then filtered. The
obtained residues were sintered at 973 and 1373 K for 3 h in a muffle furnace. To obtain the
desired grain size, the obtained silica powder was pulverised using a milling process.

2.2. Characterisation of nano silica powder

EDS (JED 2300, JEOL) analysis was carried out on the prepared samples for qualitative
elemental analysis. FTIR (Spectrum 100, Perkin Elmer, USA) was used to confirm the silica
functional group. The solid precipitate obtained from rice husk was dried under ambient
conditions and then crushed into powder. The obtained powder was mixed with potassium
bromide in 1:100 weight ratio and the pellets made from this mixture were used to record the IR
spectra in the range of 4000–400 cm1.
XRD patterns of the obtained silica powder were recorded using a powder X-ray
diffractometer (X’ Pert Pro, PANalytical, The Netherlands) with Cu-K (wavelength 1.5406 Å)
as a radiation source. The average crystallite size of the nano silica powder was calculated from
XRD pattern by using the Scherrer’s equation [25]:
0:94 
Dp ¼ ð3Þ
1=2 cos 
where Dp is the size of the particle,  the wavelength of X-ray, 1/2 the wavelength of full width
half maximum and  the peak position.
A TEM study was made to examine the morphology and particle size of the nano silica
powder (Philips, CM 200, USA). TEM images were formed using transmitted electrons having
magnification up to 1,000,000 X with a resolution better than 10 Å. The observed images were
resolved over a fluorescent screen or a photographic film.
The PSA (Nanophox, Sympatec, Germany) was used to measure the size distribution of the
particles using dynamic light scattering principle operating with a three-dimensional photon
cross-correlation technique in the range of 1–10,000 nm. The SSA of the prepared nano silica
powder was measured using BET surface area analyser (Autosorb AS-1 MP, USA). The sample
was degassed at 568 K for 3 h and the physi-sorption analysis was carried out with nitrogen gas
as an adsorbate and liquid nitrogen as a coolant. The multi-point BET correlation technique
was used to measure the SSA of the nano silica powder.

3. Results and discussion

A simple, economically viable and more convenient method has been developed to synthesise
highly pure nano silica powder using alkaline extraction followed by acid precipitation method.
Conventionally, nano silica powders are prepared using the decomposition of RHA in an
oxidising atmosphere or using high-energy inputs [19–22]. Hence, in this investigation a new
approach is adopted to produce high-purity nano silica powders using the decomposition of
RHA without an oxidising atmosphere followed by alkaline extraction – acid precipitation
method.
The production of highly pure nano silica powder is possible because of the strict adoption
of the following purification parameters while the synthesis is being done: first, rinsing the rice
husk thoroughly with distilled water could remove dust and other impurities; second, moderate
thermal treatment (973 K) in an inert atmosphere could remove even more inorganic
contaminants through decomposition; third, washing RHA before alkali extraction could
avoid impurities; fourth, leaching RHA with a 6 N HCl solution removes the metallic impurities;
fifth, repeated washing of RHA with warm distilled water until the filtrate is free from acidic
impurities; finally, purifying RHA by an alkaline extraction with different NaOH treatment
 Journal of Experimental Nanoscience 275

(0.5, 1, 1.5, 2 and 2.5 N) and rinsing the silica powder with hot water eliminates carbonates or
hydroxides of alkali metal, such as sodium.

3.1. Effect of concentration of NaOH on high-purity nano silica powder

To evaluate the effect of purification parameter and to confirm the presence of silica, EDS
analysis was carried out on nano silica powder for 0.5, 1, 1.5, 2 and 2.5 N NaOH treatments.
NaOH has an effect on the production of high-purity nano silica powder from RHA and the
influence of NaOH on purity is summarised in Figure 1(a)–(e). Figure 1(d) shows the EDS
pattern of nano silica powder at 2 N NaOH purification treatment. Majority of the elements
present are silicon and oxygen with some impurities such as sodium and carbon. The EDS
pattern of nano silica powder at 2.5 N NaOH purification treatment is shown in Figure 1(e). The
2.5 N NaOH purified nano silica powder predominantly contains elements such as Si and O. The
observed Si and O peaks confirm the presence of silica. The purified nano silica powder contains
66.29 wt% of silicon and 33.71 wt% of oxygen. It is inferred that the actual composition of
silicon in silica is 46%. The observed EDS result shows that the sample contains 66.29wt% of
silicon. It can be confirmed from EDS analysis that the sample contains more than 99% purity
of silica with free silicon. In addition, the EDS measurement of purified silica powder shows that
the content of Si and O is, respectively, 99.9 (% in wt%) and 99.9 (% in at%). The above-
mentioned results further indicate the absence of other elements such as Na and C, which, in
turn, confirms the formation of pure silica structures.
In addition, the major chemical groups present in the nano silica powder at 2 and 2.5 N
NaOH purification treatments have been identified from the FTIR spectra. Figure 2(a) shows
the FTIR spectrum of nano silica powder at 2 N NaOH purification treatment. The broad
absorption peaks between 452 and 951 cm1 are because of the silica structures and the other
peaks observed in the range of 1281–2428 cm1 are because of impurities such as carbonate and
sodium groups. On the other hand, at 2.5 N NaOH treatment, the sodium and carbonate groups
were absent in the FTIR spectrum of pure nano silica powder, as is evident from Figure 2(b).
The strong absorption peaks absorbed at 497, 623 and 795 cm1, respectively, indicate Si–O–Si
bending, Si–H and symmetric Si–O–Si stretching modes of vibrations. Thus, it is confirmed that
one can produce a highly pure nano silica powder from RHA using 2.5 N NaOH purification
treatment. Figure 3(a) shows the Raman spectra of nano silica powder at 2 N NaOH
purification treatment. The presence of broad peaks indicates the formation of silica along with
other impurities. In contrast, Figure 3(b) and (c) show the Raman spectra of pure nano silica
powder at 2.5 N NaOH purification treatment, sintered at 973 and 1373 K, respectively. The
characteristic sharp silica peak observed at 220 and 420 indicates the structure of the cristobalite
silica phases [26].
The studies at 2 and 2.5 N NaOH purification treatments of EDS, FTIR and Raman spectra
show that the purification treatment at 2.5 N NaOH is valid to achieve high-purity silica
powders. The conditions necessary for achieving high-purity nano silica include the optimum
time, number of washing cycles, temperature and concentration of NaOH solutions. The purity
of silica increases when the number of cycle increases. However, the enhancement in the purity
reaches the maximum when the sodium content in the silica is completely removed. The
optimisation of washing has been performed with respect to the content of sodium present in the
product. All these parameters prevent the resulting nano silica powder from both impurities and
larger particle sizes. Hence, the above purification treatment is more essential and viable for
obtaining high-purity nano silica powder from RHA. Following this procedure, 99.98% pure
silica can be obtained.
 276 R. Yuvakkumar et al.

Figure 1. EDS pattern of nano silica powder (a) 0.5 N, (b) 1 N, (c) 1.5 N, (d) 2 N and (e) 2.5 N NaOH purification treatments.
 Journal of Experimental Nanoscience 277

(a) (b)

Transmittance (%)
Transmittance (%)

2428

2074

951
1641

796
1389
1281

452

497
623
795
3000 2500 2000 1500 1000 500 3000 2500 2000 1500 1000 500
–1 –1
Wavenumber (cm ) Wavenumber (cm )

Figure 2. FTIR spectrum of nano silica powder (a) 2 N and (b) 2.5 N NaOH purification treatments.

Figure 3. (Colour online) Raman spectra of nano silica powder (a) 2 N NaOH purification treatment, (b)
and (c) 2.5 N NaOH purification treatment sintered at 973 and 1373 K, respectively.

Various classic methods have been proposed to obtain bulk silica powders from RHA
[13–18], though these models unpredicted the step-by-step procedure to obtain pure silica
powders. Based on the classic studies, in the present investigation, a new methodology has been
proposed to produce highly pure nano silica powder from RHA employing the above-
mentioned purification parameters. The purity, particle size and surface area values of nano
silica powder obtained in this investigation is compared with the conventional methods [19–22]
and is given in Table 1 for easy understanding.
278 R. Yuvakkumar et al.

Table 1. Characteristic comparison of the prepared nano silica with conventional nano silica.

Nano silica product Purity (%) Average particle size (nm) Surface area (m2 g1)

[19] 95 60 235
[20] – 50–70 –
[21] 99 33–46 260
[22] 95 26 250
Present study 99.98 25 274

(b)
Intensity (a.u.)

(a)

0 10 20 30 40 50 60 70 80
2θ (Degree)

Figure 4. XRD pattern of pure nano silica powder (a) sintered at 973 K and (b) sintered at 1373 K.

The purity (99.9%), particle size (around 25 nm) and BET surface area (274 m2 g1) values
of 2.5 N NaOH-treated nano silica are found to be enhanced in all aspects than the reported
values. It is inferred from the above studies that 2.5 N NaOH treatment is best suited for the
synthesis of high-purity nano silica powders with a low-synthesis technique. The concentration
of NaOH had strong effect on the dissolution, particle size and surface area of silica and also
removed some impurities which were not dissolved from the main product.
The XRD patterns of the obtained pure nano silica powder were sintered at 973 K, as shown
in Figure 4(a). The characteristic broad silica peak observed at 2 ¼ 22 indicates the presence of
amorphous silica. The absence of sharp peaks at this temperature indicates the absence of
crystallinity. In contrast, to achieve the crystalline phase and to measure the crystallite size of the
pure nano silica, the product is sintered at 1373 K. The crystalline phase is evident from
the sharp peaks that are observed (Figure 4b). The average crystallite size calculated from the
broadening of the corresponding sharp peaks by the Scherrer formula is 25 nm. The sharp peaks
observed from the XRD pattern reveal the formation of cristobalite structures [27]. A similar
observation was made in the Raman study.
 Journal of Experimental Nanoscience 279

Figure 5. TEM image of pure nano silica powder.

6
Density distribution (q)

0 20 40 60
Particle size (nm)

Figure 6. Particle size distribution of pure nano silica powder.

In addition, TEM and PSA studies have been carried out on the sintered samples at 1373 K
to correlate the particle size of the obtained pure nano silica powder. The TEM image of the
nano silica powder is shown in Figure 5. The obtained nano silica powder is uniform and
agglomerated. The shape of the silica grains is spherical with an average homogeneous
particle size distribution of about 25 nm, which is in good agreement with the average crystal
size estimated from XRD pattern. Further, the particle size distribution of the nano powder was
measured using photon cross-correlation spectroscopy. The particle size distribution curve of
the nano silica powder is shown in Figure 6. The average particle size distribution of the
product obtained by the present process is 29 nm (designated as d10% ¼ 24.19, d50% ¼ 29.17
280 R. Yuvakkumar et al.

4.0

3.5

1/(W((P0/P)-1))
3.0

2.5

2.0

1.5

1.0
0.10 0.15 0.20 0.25 0.30
(P/P0)

Figure 7. BET surface area plot of nano silica powder.

and d90% ¼ 35.18 nm). The particle size obtained from PSA is reasonable and is consistent with
the results of TEM and XRD.
The SSA of the material was measured using multiple-point BET surface area analyser. The
SSA of the nano silica powder is approximately 274 m2 g1 with an average pore diameter of
approximately 1.46 nm (Figure 7). BET analysis confirmed that the obtained nano silica powder
is a microporous material with high SSA.
The results that are obtained by the proposed method confirm the quality of the production
of high-purity nano silica powder from rice husk. Most of the other conventional methods are
more expensive and require high-energy inputs. To overcome this and to produce high purity,
the proposed method can be implemented and is suitable for producing high-purity nano silica
powder from rice husk using a simple chemical method.

4. Conclusion
Highly pure nano silica powder is synthesised from rice husk using a simple precipitation
technique. The nano silica powder that is obtained is characterised in terms of its content,
particle size, SSA and pore diameter. The 2.5 N NaOH treatment resulted in high-purity silica
content. The purity of silica that is obtained is about 99.9% (wt%) and 99.9% (at%) with an
average particle size of 25 nm. The successful synthesis of high-purity nano silica powder is
possible by using the method described in this study.

Acknowledgements
The authors are very thankful to Defence Research and Development Organisation
(DRDO), New Delhi, for the financial support to carry out this project (ERIP/ER/0705077/M/01/1015
dt. 20.11.07).
 Journal of Experimental Nanoscience 281

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