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Synthesis of Magnesium Oxide Nanoparticles by Sol-Gel Process

Article  in  Materials Science Forum · October 2007

DOI: 10.4028/www.scientific.net/MSF.558-559.983

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Materials Science Forum Vols. 558-559 (2007) pp. 983-986
online at http://www.scientific.net
© (2007) Trans Tech Publications, Switzerland

Synthesis of magnesium oxide nanoparticles by sol-gel process

Rizwan Wahab1,a, S.G. Ansari1,b, M.A. Dar1,c, Y.S. Kim1,d and H.S. Shin 1,e
1
Thin film Technology laboratory, School of Chemical Engineering, Chonbuk National University,
Chonju, S.Korea, 561-756
a
rizwan@chonbuk.ac.kr, bpiezo2k@chonbuk.ac.kr, cmushtaq@chonbuk.ac.kr
d
kyscjb@chonbuk.ac.kr, ehsshin@chonbuk.ac.kr

Keywords: MgO, Sol-gel, Cubic nanoparticles

Abstract. Cubic shaped Magnesium oxide nanoparticles were successfully synthesized by sol-gel
method using magnesium nitrate and sodium hydroxide at room temperature. Hydrated Magnesium
oxide nanoparticles were annealed in air at 300 and 500ºC. X-ray diffraction patterns indicate that
the obtain nanoparticles are in good crystallinity, pure magnesium oxide periclase phase with (200)
orientation. Morphological investigation by FESEM reveals that the typical sizes of the grown
nanoparticles are in the range of 50-70nm. Powder composition was analyzed by the FTIR
spectroscopy and the results confirms that the conversion of brucite phase magnesium hydroxide in
to magnesium oxide periclase phase was achieved at 300ºC.The Thermo-gravimetric analysis
showed the phase transition of the synthesized magnesium oxide nanoparticles occurs at 280-300ºC.

Introduction

Nanoparticles have attracted a great attention in recent years because of their unique
physical and chemical properties such as high strength with good thermal conductivity, higher
damping property and mechanical stability [1]. The high surface reactivity, high chemical and
thermal stability of MgO makes it a promising material for the application in sensors, catalysis,
paint and additives etc [2-8]. Magnesium oxide nanoparticles and micro particles are largely used as
a reinforcing reagent, as well as a component in super conductors [9]. Due to the high surface
reactivity, highly chemical and high thermal stability with the catalytic properties, the magnesium
oxide nanoparticles have particular interest [10]. The vast applications of magnesium oxide
nanomaterials inclined to work on this material. Various kinds of fabrication techniques are
employed to grow magnesium oxide nanoparticles such as vapor-liquid-solid (VLS), chemical
vapor deposition (CVD), plasma enhanced chemical vapor deposition (PECVD), Pulsed laser
deposition (PLD), laser ablation, molecular beam epitaxy (MBE) and sputtering method have been
frequently employed [4]. All these methods require high temperature or sophisticated and/or
expensive instruments. The chemical route, Sol-gel processes, has become a promising option for
the synthesis and large-scale production of nanostructured materials as well as magnesium oxide. In
this paper, we present synthesis and characterization of crystalline cubic shaped MgO nanoparticles
by sol-gel method at room temperature.

Experimental

Magnesium oxide nanoparticles were synthesized using magnesium nitrate (MgNO3.6H2O) as

a source material with sodium hydroxide. All the chemicals used for this synthesis were purchased
from Aldrich Chemical Corporation and used without further purification. For the typical
experimental procedure; 0.2M magnesium nitrate (MgNO3.6H2O) was dissolved in 100 ml of
deionized water. 0.5M sodium hydroxide solution was added drop wise to the prepared magnesium
nitrate (MgNO3.6H2O) solution while stirring it continuously. White precipitate of magnesium
hydroxide appeared in beaker after few minutes. The stirring was continued for 30 minutes. The pH
of the solutions was 12.5, as measured by the expandable ion analyzer (EA 940, Orian, Korea). The
precipitate was filtered and washed with methanol three to four times to remove ionic impurities

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984 Recrystallization and Grain Growth III

and then centrifuged for 5 minutes at 5000 rpm/min and dried at room temperature. The dried white
powder samples were annealed in air for two hours at 300 and 500ºC. The morphological
investigation was carried out by the field emission scanning electron microscopy (FESEM, Hitachi
S4700). The crystallinity and crystal phases were determined by X-ray powder diffractometer
(Rigaku, XRD) with CuKα Radiation (λ=1.54178Ǻ) with Bragg angle ranging from 30 to 80°.
Samples composition of the synthesized magnesium oxide nanoparticle was analyzed by the Fourier
transform infrared (FTIR) spectroscopy (Bomem, Model DA8-12, Canada) in the range of 400-
4000 cm-1. Thermo gravimetric (TG) and differential scanning calorimetry (DSC) were conducted
by TGA 2050 thermo-gravimeter and DSC 2910 differential scanning calorimeter with the heating
rate of 20º and 10º min-1 respectively.

Result and discussion

Fig1 (a) and (b) shows the FESEM images of

as grown magnesium oxide nano particles at room
temperature. The particles appear spherical in shape,
and agglomerated. High-resolution image of
annealed powder at 300˚C (Fig 1(c) and (d)) clearly
shows the cubic form of separated magnesium oxide
nanoparticles, with particle size of about 50-60 nm.
Annealing at 500˚C, results in further agglomeration of
the particle as well as deterioration of the spherical
shape. The cor responding SEM images are shown in
Fig. 1(e) and (f), where elongated, spherical and cubic
shaped nanoparticles of magnesium can be seen.
Fig 2(a) shows the X-ray diffraction spectra of
as grown magnesium oxide nanoparticles at room
temperature. From the peak width and intensity we can
easily see that the smaller particle size and better Fig.1 (a) and (b): as grown magnesium oxide
crystallinity.Fig.2(b)and (c)shows the X-ray nanoparticles; (c), (d), (e) and (f) shows the cubic
diffraction pattern of the samples annealed at 300 and form of magnesium oxide nanoparticles annealed
500°C for two hours in air. The observed diffraction at 300ºC and 500ºC for two hours in air.
peaks are well matched with the typical
single crystalline periclase phase of bulk (c) calcined at 500 C
o

MgO and are also in good agreement with

the JCPDS file for MgO (JCPDS, Card No.
36–1451). No other peaks were detected
Intensity(a.u.)

o
in the spectrum within the detection (b) calcined at 300 C

limit of the X-ray diffraction instrument,

Mg(O2)2(202)

indicating the purity of the synthesize

MgO (200)

powder. The (200) intense and sharp

Mg(O2) 2(413)
Mg(O2)2(312)

MgO (220)
MgH2(111)

(a) As grown
peak of periclase phase in the diffraction
MgO(111)

MgH2(221)
MgO(222)

MgO(511)

MgO(311)
MgH2(200)

spectrum shows the high-crystallinity of the

Mgo(222)

product.
*

*
*
*

The composition of the sample was

*

analyzed by the FTIR measurement. The 30 40 50 60 70 80

synthesized powder was mixed with KBr 2θ (Degree)
and the pellet of the mixture was used for Figure 2(a): X-ray diffraction spectra of (a) as grown magnesium
infrared (IR) spectroscopic measurement at oxide nanoparticles, annealed at (b) 300 and (c) 500°C for two
room temperature while the wavelength was hours in air* marked peaks are unidentified
varied from 400 to 4000 cm-1. Fig 3(a) shows the spectra of as grown powder sample. The
absorption band at 1630-1640 cm-1 indicates the bending mode of vibration in water (HOH) and the
 Materials Science Forum Vols. 558-559 985

broad and shallow band observed in the region

between 3000-4000 cm-1 shows the stretching mode (c)
of vibration in hydroxyl group (O-H). The peak at
3700 cm-1 is due to the O-H vibration of brucite

Transmittance (a.u.)
phase of Mg(OH)2 .The broad spectrum between (b)
3300cm-1 to 3600 cm-1 shows the formation of
MgO [12]. Narrow peak of magnesium hydroxide
at 3700 cm-1 disappeared in Fig 3 (b) and 3(c), (a)
which is due to calcinations of the sample at 300
and 500°C. It clearly indicates that the brucite phase
of magnesium hydroxide is converted into the 4000 3500 3000 2500 2000 1500 1000 500
periclase phase at two different annealing -1
Wavenumbers (cm )
temperatures, analogous to X-ray diffraction results.
Thermo gravimetric analysis is a technique Fig. 3: FTIR spectra of (a) as grown magnesium
°
by which we can measures the mass loss with 100
respect to temperature. Fig. 4(b) shows the weight
loss of the as grown powder sample. Primary
90
weight loss of ~ 11.92% was observed at 103°C
%Weight loss

due to the solvent evaporation. Phase transition solvent evaporation point

80
is found to occur at about 300°C indicating the
transition from magnesium hydroxide to phase transition point

magnesium oxide with weight loss of ~ 15- 70

19%.
60
DSC was carried out in the range of 30°C to
Formed magnesium oxide
350°C temperatures. Fig.4(b) shows a broad 500 200 400 600 800
exothermic signal was observed between 150°C 0
Temperature C
and 300°C.The broad exothermic signal at 150°C
of primary weight loss is assigned to the Fig.4(a):Thermo-gravimetric spectrum of as grown
magnesium oxide.
desorption of physically adsorbed water. The XRD
spectrum (fig. 2b) of the sample annealed at 300ºC
support the DSC observation, as the peaks of
MgH2 disappears after calcination at 300°C.
Exo and Endo

An exothermic signal with secondary weight

loss was observed in between 280°C to 300°C,
which is due to the phase transition of
magnesium hydroxide powder in to
magnesium oxide.

Conclusion

In summary, brucite and periclase phase of 50 100 150 200 250 300 350
0
magnesium oxide nanoparticles were synthesized Temperature C
by the sol-gel method using magnesium nitrate Fig. 4(b): Differential scanning calorimatery of as
(MgNO3.6H2O) as a source material with sodium grown magnesium oxide.
hydroxide. The dried white gel was annealed in air for two hours at 300 and 500ºC. SEM
observations clearly show the cubic form of separated magnesium oxide nanoparticles of about 50-
60 nm in size. Annealing at 500˚C, results in further agglomeration of the particle as well as
deterioration of the spherical shape. XRD measurements revealed typical single crystalline periclase
phase of bulk MgO. No other peaks were detected in the spectrum within the detection limit of the
X-ray diffraction instrument, indicating the purity of the synthesize powder. FTIR measurement
 986 Recrystallization and Grain Growth III

shows that the brucite phase of magnesium hydroxide is converted into the periclase phase at the
two different annealing temperatures, TGA and DSC indicates the transition from magnesium
hydroxide to magnesium oxide. This method is found to be a mild and efficient route for the large-
scale industrial production of fine magnesium oxide nanoparticles without any template or
expensive chemicals.

Acknowledgement

S G. Ansari acknowledges KOSEF and KRF for Brain-Pool fellowship. This work was supported
by KMOST (research Grant No. 2004-01352), KOSEF (research Grant No. R01-2004-000-10792-
0) and by the grant of Post Doc program, Chonbuk National University (01-the second half term of
2006). Authors would like to thank the Korea Basic Science Institute (Jeonju branch) for the use of their
FESEM.

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