Proceedings of the International Conference on Materials, Design and Manufacturing Process
ICMDM 16
SYNTHESIS OF MgO NANOPARTICLES USING SOL GEL METHOD FOR POROUS
WICK STRUCTURE OF A FLAT PLATE HEAT PIPE
1,*
P.Pandiyaraj
Research Scholar, Dept. of MechanicalEngg
Chennai, Tamilnadu, India
3
P.Saravanan
Research Scholar, Dept. of Industrial Engg
Chennai, Tamilnadu, India
ABSTRACT
In this research, porous MgO particles were prepared
through wet chemical method using magnesium nitrate as
Precursor and sodium hydroxide as a reducing agent. The
materials obtained by Sol gel method were subsequently
annealed at 300 to 500 C for 3hours to improve the
crystallinity and phase purity. Then Obtained MgO
nanoparticles were characterized by UV absorption
spectroscopy, powder XRD, infrared spectroscopy, scanning
electron microscopy (SEM). The precipitated white gel was
annealed in atmospheric air for more than two hours at 200C
and 400C. Annealing at 400C makes agglomeration of the
particle as well as affects its spherical shape. XRD results
revealed uneven single crystalline periclase phase of MgO.
More number of sharp peaks was not detected, thus indicating
the purity of the annealed powder. FTIR measurement reveals
that the brucite phase exists in magnesium hydroxide is
transformed into the periclase phase at different annealing
temperatures (200 and 400C). The SEM image shows that the
annealed MgOnanomaterials are highly porous in nature and
highly agglomerated too. SEM observations partially show the
cubic form of isolated magnesium oxide nanoparticles. The
individual particle size of MgO was not seeing properly in
SEM results. The present results prove that the sol gel
technique can produce the materials with high crystallinity and
porosity. So far, this is the initiative report on the synthesis of
MgO Nanoparticles by Sol Gel technique followed by
Annealing for a Porous Body material of Flat heat Pipe.
INTRODUCTION
Magnesium oxide (MgO) is a versatile oxide material, with
high melting point (2850C) and high boiling point (3600C);
thereby it is thermally so stable. It has the same structure
as NaCl, therefore Ions are strongly attracted to each other. So
it requires far more energy to pull aside, hence enough evidence
of MgO generally has a high melting point, nearly thrice the
melting point of sodium chloride. This strong attraction of ions
February 17-19, 2016, Chennai, INDIA
4977
2
A.Gnanavel babu
Associate Professor, Dept. of Industrial Engg
Chennai, Tamilnadu, India
is exact verdict to confirm magnesium oxide is minimally
soluble than sodium chloride. Hot magnesium allows suitable
energy for oxygen molecules to fragment, transgressing the
very strong O=O double bond. Individual magnesium atom
supplies two electrons to an oxygen atom, hence magnesium
oxide contains Mg2+, and oxide, O2 ions. Due to its high
melting point, magnesium oxide possesses inflexible properties,
so it can be used as a body material, furnace and crucibles. In
addition, MgO compounds prepared by those conventional
methods often yields a relative small surface area and hence
shows low reaction activity [1]. It has been reported that the
catalytic properties of sol-gel MgO catalyst strongly depend on
the crystallite size, surface area, structure defects and acid-basic
concentration. In nano size, to make MgO nanoparticles, wet
chemical and sol gel techniques are followed with suitable
reducing agent and further treated to annealing process [10].
Recently, sol-gel process has assumed a special significance for
synthesis MgO compounds because it is simple, cost effective,
and capable of yielding unique properties such as large surface
area-to-volume ratio and narrow particle size distribution at
relative low temperatures [2]. Several factors such as annealing
temperature, annealing time, pH, catalytic agents and
environment conditions drastically affect the characteristics of
the magnesium oxides [3].
EXPERIMENTAL PROCEDURE
Reagents such as, Magnesium nitrate (MgNO3.6H2O),
Sodium hydroxide (NaOH) and other chemicals are used in the
synthesis of MgO nanoparticles [4]. De-ionized water was
prepared in the laboratory to be used as solvent. Magnesium
oxide nanoparticles were synthesized by magnesium nitrate
(MgNO3.6H2O) as a precursor and sodium hydroxide as
reducing agent. At first, 0.2M magnesium nitrate
(MgNO3.6H2O) was completely dissolved with sonification in
100 ml of double distilled water and stirred well for 30 minutes.
Then 0.5M sodium hydroxide was dissolved in 100 ml of
double distilled water and stirred well for 30 minutes. Now
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prepared reducing agent (NaOH) is added drop wise in the
existing magnesium nitrate (MgNO3.6H2O) solution, and stirred
continuously. Later white precipitation of magnesium
hydroxide is formed. The stirring was continued for 30 minutes.
The precipitate was cleaned with filtration and thoroughly
washed with methanol to remove ionic impurities and then the
powder samples were annealed in atmospheric air for more than
two hours at 200C and 400 C [5]. First of all, to confirm the
presence of Magnesium oxide nanoparticles, it is analyzed
under UV-Visible spectroscopy (JASCO V 650). The
crystallinity and crystal phases are determined by X-ray powder
diffraction (XRD). Then the synthesized magnesium oxide
nanoparticle was also analyzed using the Fourier transform
infrared spectroscopy (FT-IR).

Figure 2. UV Spectroscopy of MgO

Figure 1. Preparation Chart of MgO Nanoparticles
RESULTS AND DISCUSSIONS
i. UV SPECTROSCOPY
Magnesium oxide nanoparticles were prepared by
electrochemical route using sol-gel method at room temperature
and analysed by UV-Visible spectroscopy (JASCO V 650).
Figure 2 represents the optical absorption spectra of
Magnesium oxide respectively. The characteristic SPR
symmetric of 300nm with an absorbance of 0.9 obtained for red
colour magnesium oxide nanoparticles. These absorbance
wavelengths of magnesium oxide nanoparticles are compared
to the earlier reported paper. The reported paper was obtained at
the absorption wavelength is 320nm, 300-350nm the results
obtained.A Magnesium oxide nanoparticles is obtained at
300nm and it is compared to the earlier reported paper. The
presence of silver, aluminium and copper nanoparticles was
thus confirmed. The synthesized MgO nanoparticles exhibited a
red colour in aqueous solution, due the excitation of surface
Plasmon resonance.
ii. FT-IR ANALYSIS
The FT-IR spectra of MgO taken after the synthesis of
nanoparticles at 200C and 400C were analyzed for the
determination of possible functional groups which leads to
formation of metal nanoparticles. The FTIR spectrum for the
annealed MgOnano powder is shown in Figure. From FT-IR
results, the stretching vibration mode for the MgOMg
compound was in the range of 433575 cm1 as a broad band.
Two different bands are found at the wave number ranges of
11221208 cm1 and 13881462 cm1 and they are
recognized to the bending vibration of completely absorbed
water molecule and surface hydroxyl group (OH),
correspondingly [7] . A unique broad vibration band was found
in the wavenumber range 3425 3698 cm1 because of OH
stretching vibration of aerial absorbed water molecule and
surface hydroxyl group [9]. The FT-IR absorption peak was
found at the wavenumber 1493 cm1, it allots the asymmetric
stretching of the carbonate ion [7].
Figure 3. FTIR Graph of Annealed MgO
iii. TGA/DTA
Thermal decomposition behavior of the Annealed MgO
was investigated using TGA/DTA. The weight loss occurred till
680C for the MgO. The exothermic peak is observed at 607C.

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The organic residues are disappeared at a temperature 567.25C
and 586.37C. From the TGA curve, the complete weight loss
is observed at 676.48C.

Figure 6. XRD Graph of MgO

v. SEM Analysis
From the SEM photographs (Fig 7), it can be observed that
MgO nanoparticles are randomly distributed, thereby
suggesting that the material behaves homogeneously at macro-
length scales [8]. The SEM images are taken in many
magnifications. The SEM results show that the annealed
MgOnanomaterials are relatively porous and highly
agglomerated with the nano entities. Thus the particle size of
MgO could not be seen accurately from the present SEM
results
Figure 4. TGA/DTA Analysis of Annealed MgO

iv. XRD Analysis

The powder XRD was set in the 2 range between 20 to
80 using Cu K radiation. The powder XRD patterns were
taken for both MgO nanoparticles as before annealed and after
annealed. From these XRD patterns, we found that the annealed
material was crystallized and occurs in single phase with cubic
symmetry. The Bragg reflections such as (111), (002), (202),
(113), and (222) are seen in the 2 range between 20 and 80.
All reflections are sharp with slight broadening. These reflect
the crystalline nature of MgOnanopowder. The average
crystalline size of 22 nm is obtained for the annealed
nanocrystallineMgO powder from the Debye Scherrer formula
using the XRD powder data [6].
Figure 7.a. SEM images of Annealed MgO at 500m
Counts
A1

200

100

0
20 30 40 50 60 70
Position [2Theta] (Copper (Cu))

Figure 5. XRD of Annealed MgO

Figure 7.b. SEM images of Annealed MgO at 20m

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Figure 7.c. SEM images of Annealed MgO at 5m
Figure 7.d. SEM images of Annealed MgO at 2m
CONCLUSIONS
The method Adopted to Prepare MgO nanoparticles is found to
be safe and inexpensive, considering the explosive nature of
Magnesium. From the above XRD results, it is evident that
Mgo has crystallinity and purity. The particle size are found in
the range of 30-40 nm. Also from the SEM results, MgO
nanoparticles are highly agglomerated and porous. By applying
suitable pressure and temperature, this would be better suited
for manufacturing porous element like wick of the flat plate
heat pipe which the researchers are aiming at. The
characteristics of the MgO nanoparticles will also be suited for
applications like body material, Fireproofing walls, refractory
materials, Furnaces and crucibles by proper compacting with
temperature.
ACKNOWLEDGMENTS
This research work is supported by the Department of
Mechanical engineering, CEG Anna University, Chennai.
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