See discussions, stats, and author profiles for this publication at: https://www.researchgate.

net/publication/230750666

Synthesis of MgO Nanopowder viaNon Aqueous Sol–Gel Method

Article  in  Journal of Computational and Theoretical Nanoscience · July 2012

DOI: 10.1166/asl.2012.2190

CITATIONS READS
13 1,472

3 authors:

Taimur Athar Abdul Hakeem Deshmukh

Indian Institute of Chemical Technology Polish Academy of Sciences
68 PUBLICATIONS   401 CITATIONS    40 PUBLICATIONS   182 CITATIONS   

SEE PROFILE SEE PROFILE

Waqar Ahmed
University of Lincoln
362 PUBLICATIONS   4,223 CITATIONS   

SEE PROFILE

Some of the authors of this publication are also working on these related projects:

I am researching now on Boswellia sacra and looking at the anticancer activity of this omani frankincense. View project

Characterisation of nano-engineered dental implants View project

All content following this page was uploaded by Abdul Hakeem Deshmukh on 01 June 2014.

The user has requested enhancement of the downloaded file.

 RESEARCH ARTICLE
Copyright © 2012 American Scientific Publishers Advanced Science Letters
All rights reserved
Printed in the United States of America
Vol. 5, 1–3, 2012

Synthesis of MgO Nanopowder via

Non Aqueous Sol–Gel Method
Taimur Athar1 , Abdul Hakeem1 , and Waqar Ahmed2 ∗
1
Indian Institute of Chemical Technology, Tarnaka, Hyderabad (A.P.), 500-007, India
2
Institute of Nanotechnology and Bioengineering, University of Central Lancashire, United Kingdom

Magnesium Oxide (MgO) is an attractive material for a wide range of application such as catalysis, treatment
waste and an additive to paints, refractory materials and superconductive materials. It yield significant advantage
when it is manufactured and used on a nanoscale dimensions. In this study cubic MgO nanoparticles were
prepared by using non-aqueous sol–gel process with good morphology and with limited surface area properties
and monodispersity. The nanoparticle was characterized by various analytical techniques such as TEM, SEM,
XRD, TGA/DTA, FT-IR and Raman spectroscopy. The average particle size with 43 nm and surface area of
2.81 m2 /g was obtained. The non-aqueous process offers the better understanding for controlling the reaction
mechanism at a molecular level with high cyrstallinity and well defined uniform morphologies.

Keywords: Sol–Gel, Monodispersity, Surface Area, Uniform Morphologies.

1. INTRODUCTION 4 cm−1 resolution. Raman spectroscopy were recorded by using

From ancient times MgO plays a very prominent role based on
surface properties. It is used in catalysis, toxic waste remediation,
or as an additive in refractory materials, paints and superconduc-
tor materials based on its versatile basic properties.1–3 It is used
in many organic reactions,4 as a supporting catalyst due to their
adsorbent tendency with an enhanced surface area and with their
intrinsically high surface reactivity.5–7 Many synthetic approach
has been applied for the synthesis of ultra-pure MgO such
as Vapor phase oxidation,8 Hydrothermal,9 High temperature
solid state synthesis,10 alkoxide based preparation,11 Micro wave
irradiation12 and sol–gel synthesis.13 Among all these techniques
non aqueous sol–gel technique is preferred because it is easy
to control particle properties via soft chemical approach. Simple
and cost effective, eco-friendly to synthesize MgO nanoparticles
synthesis was carried out with monodispersity and with limited
uniform particle size, shape and porosity having high surface
chemical reactivities.
2. CHARACTERIZATION OF SAMPLE
Solvents were distilled under nitrogen prior to use. Starting mate-
rials were purchased from Aldrich and used as such. Analysis
was carried out at room temperature under anhydrous condi-
tions. FT-IR spectra were recorded on a Bruker spectrometer
(VERTEX 80v) in the 4000–400 cm−1 range. The samples were
analyzed as such, by collecting and averaging 64 scans with
∗
Author to whom correspondence should be addressed.
Lab RAM HR800 using 632 nm Laser as the excitation source.
X-ray studies was obtained on a Rigaku diffractometer (DMAX-
2500) using CuK radiation ( = 0154 nm), scanning was per-
formed from 10 to 80 in 2. Thermal analysis was carried
out in flow of dried air (100 cm3 /min) on a thermo balance
(TA Instrument, SDT-2960). The programmed heating rates were
10  C/min and the sample was heated from room temperature
to 1000  C. X-ray diffraction and electron microscopic studies
helps to better understand the structural changes that take place
in thermal treatment. Transmission electron microscopic images
were taken by using a JEOL electron microscope (JEM-2100)
equipped with a slow-scan CCD camera operating at 200 kV.
TEM specimens were obtained from the homogenous colloidal
solution. The solutions were dropped on a copper grid coated
with an amorphous carbon film and subsequently dried in vac-
uum. The Brunauer–Emmett–Teller (BET) was analyzed by using
an automatic physico-sorption analyzer (Micromeritics ASAP
2020).14–15 All samples were degassed at 80  C prior to nitrogen
adsorption measurements.16
3. EXPERIMENTAL METHODS
Synthesis of MgO nanoparticles was carried out via non aqueous
sol–gel process:
Alkali solution of toluene (A.R Aldrich) was prepared by dis-
solving 2 gm of KOH (35.71 mmol) pellets in 20 ml of toluene
with vigorous stirring for 12 hrs. Then followed by addition of
3 gm (14.75 mmol) of MgCl2 · 6H2 O (A.R Aldrich) into this

Adv. Sci. Lett. Vol. 5, No. xx, 2012 1936-6612/2012/5/001/003 doi:10.1166/asl.2012.2190 1

RESEARCH ARTICLE
Fig. 1. XRD spectum of MgO.
solution and then refluxed for 3 hrs. The compound was sepa-
rated out by filtration, and then washed thoroughly with distilled
water (till filtrate becomes neutral). The compound was oven
dried for 6 hrs at 100  C followed by calcination at 550  C (with
an increase in temperature of 2  C/min for 4 hrs) was carried out
in atmospheric condition. White fine powder was obtained with
85% yield.
4. RESULTS AND DISCUSSION
In non aqueous sol–gel process the formation of metal oxide
nanoparticles take place by providing oxygen from alkali hydrox-
ide or by any organic constituents present in precursor.
C6 H6
MgCl2 · 6H2 O + 2KOH −−−−→ MgO + 2KCL + 7H2 O
Hexane
The characterization was successively carried out with the help
of FT-IR by observing significant frequencies at 400–4000 cm−1
that confirm the formation of MgO nanoparticles with size
effect.17 A symmetric frequency observed at 522 cm−1 and asym-
metric frequency observed at 875 cm−1 corresponds to cubic
Mg–O bond. The other peak that was observed was due to the
presence of Mg–OH bond. The presence of OH peak occurs
due to absorption of water at 3000–38000 cm−1 during sample
preparation. With an increase of the calcinations temperature the
absorption peaks are intensified thereby supporting the formation
of pure phase.
4.1. XRD Analysis
Wide-angle XRD analysis as shown below gives the information
that initially the particles are formed in amorphous phase. Dur-
ing synthesis and then subsequently heat treatment at 550  C for
Fig. 2. SEM image of MgO.
2
Adv. Sci. Lett. 5, 1–3, 2012
Fig. 3. TEM image with SAED of MgO.
4 hours (at the rate of 2  C/min) in an inert atmosphere changes
the amorphous state into crystalline phase retaining particle prop-
erties under controlled. The mean particle size was found to be
43.3 nm as calculated by using Debye-Scherrer equation.
D = K/ cos 
The peaks were assigned at (2 = 285) and (2 = 405) corre-
sponds to the synthesis of a pure cubic homogeneous particle size
and phase which corresponds to the JCPDS file [45-0946] which
is consistent with the results as reported in the literature. The
presence of intense peaks shows that the powders are crystalline
form with pure phase after high temperature treatment.
4.1.1. EDX
The presence of desired chemical composition ratio was found
to 1:1 as supported by the TEM and SAED techniques in the
calcined sample.
4.2. SEM and TEM
Scanning electron micrograph images shows that the presence
of irregular particle with micro pores has a great tendency for
agglomeration due to their surface energy leading to the forma-
tion of large surface area. The existence of big particle takes
place due to Ostwald ripening process with a limited porosity
and crystalinity.
TEM images show a spherical particle with an average size
of about 40 nm agrees well with results provided by XRD.
The d-spacing values of sample matches well with the standard
JCPDS FILE (30-0794) with clear crystalinity as supported by
SAED.
Fig. 4. Thermal analysis of MgO.
 Adv. Sci. Lett. 5, 1–3, 2012 RESEARCH ARTICLE

0.04
5. CONCLUSION
The present study shows that crystalline MgO nanopowders can
be synthesized from non aqueous sol gel process leads to the
Intensity

formation of solid takes place with yield of 85% after calcina-

0.02
tion. Non aqueous sol gel process is a cost effective with an
easy availability of raw materials which favors the scaling up of
industrial production with controlled morphology and size.
0.00

500 1000 1500 2000 2500 3000

Wavenumber(cm–1)
Fig. 5. Raman spectrum of MgO.
4.3. Thermal Analysis
Thermal analysis of MgO nanoparticles was carried out to find
the crystallinity temperature. The first weight loss occurs at
129.1  C due to vaporization of absorbed water. The second
weight loss occurs at 225.8  C it is due to removal of organic
moieties thereafter no significant weight loss was observed at
higher temperatures supporting the formation of highly crys-
talline cubic MgO at 749.8  C. Finally the formation of crys-
talline particle takes place at 860  C as supported by DSC
Thermogram due to nucleation 950.8  C.
4.4. Raman Analysis
The peaks below 1500 cm−1 is associated to D-band also known
as breathing mode. The peaks at 1500 cm−1 and 3000 cm−1 rep-
resent as a G-band. The ratio of the intensities of D and G band
(i.e., ID /IG  related to the indirect measurement of the crystallite
size and its defects. This data is consistent as reported Ref. [18].
The Raman spectrum obtained from the MgO shows a strong
peak at various region indicating the cubic structure as designated
to the tangential modes of MgO in the amorphous phase.
References and Notes
1. S. Rajagopalan, O. Koper, S. Decker, and K. J. Kiabunde, Eur. J. Chem.
8, 2602 (2002).
2. C. M. Boyapati, R. S. Mulukutla, and K. J. Klabunde, J. Am. Chem. Soc.
125, 2020 (2003).
3. J. V. Stark and K. J. Klabunde, Chem. Mater. 8, 1913 (1996).
4. H. Hideshi, Chem. Rev. 95, 537 (1995).
5. B. Q. Xu, J. M. Wei, H. Y. Wang, K. Q. Sun, and Q. M. Zhu, Catal. Today
68, 217 (2001).
6. O. B. Koper, I. Lagadic, A. Volodin, and K. J. Klabunde, Chem. Mater. 9, 2468
(1997).
7. (a) K. J. Klabunde, J. Stark, O. Koper, C. Mohs, D. G. Park, S. Decker,
Y. Jiang, I. Lagadic, and D. Zhang, J. Phys. Chem. 100, 12142 (1996); (b) K. P.
McKenna, D. Koller, A. Sternig, N. Siedl, N. Govind, and P. V. Sushko, ACS
Nano 5, 3003 (2011).
8. K. Itatani, Y. R. F. S. Howell, and A. Kishioka, J. Mat. Sci. 32, 2977
(1997).
9. (a). S. Somiya and R. Roy, Bull. Mater. Sci. 23, 453 (2000); (b). Y. Su, H. Wei,
Z. Zhou, L. Wei, Y. Zhang, Mat. Lett. 65,100 (2011).
10. V. G. Myagkov, O. A. Bayukov, L. E. Bykova, V. S. Zhigalov, and G. N.
Bondarenko, JEPT Letters 80, 487 (2004).
11. R. Zhang and L.Gao, Mater. Res. Bull. 37, 659 (2002).
12. Z. Li, Y. Liu, P. Gong, and Y. Zhai, Rare Metals 26, 476 (2007).
13. I. C Cosentino, E. N. S. Muccillo, R. Muccillo, and F. M. Vichi, J. Sol–Gel. Sci.
Tech. 37, 31 (2006).
14. S. J. Gregg and K. S. W. Sing, Academic Press, London (1982).
15. E. P. Barrett, L. G. Joyner, and P. H. Halenda, J. Am. Chem. Soc. 73, 373
(1951).
16. K. S. W. Sing, D. H. Everett, R. A. W. Haul, L. Moscou, R. A. Pierotti,
J. Rouquerol, and T. Siemieniewska, Pure Appl. Chem. 57, 603 (1985).
17. X. Ye, J. Sha, Z. Kuan, and J. Zhang, Nanostructure Mater. 8, 945 (1997).
18. B. C. Liu, B. Yu, and M. X. Zhang, Chem. Phys. Lett. 407, 232 (2005).

Received: 3 March 2011. Accepted: 25 September 2011.

View publication stats