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Materials Today: Proceedings 2 (2015) 4360 – 4368

International Conference on Nano Science & Engineering Applications. ICONSEA-2014

SYNTHESIS AND CHARACTERIZATION OF

MgONANOPARTICLES BY NEEM LEAVES THROUGH
GREEN METHOD
S Krishna Moorthya, CH Ashokb, K Venkateswara Raob*, C Viswanathana
a
Department of Nanoscience and Technology, Bharthiar University, Coimbatore, Tamil Nadu-641046, India.
b
Centre for Nano Science and Technology, Institute of Science and Technology, Jawaharlal Nehru Technological University Hyderabad,
Telangana-500085, India.

Abstract

Metal oxide nanoparticles can be used in electronics, catalysis, ceramics, petrochemical products, coatings and many other
fields such as sound-proof, light-weight, heat-insulating and refractory fibre board and metallic ceramics. Synthesis of metal
oxide nanoparticles can be done through three methods like physical, chemical, and green methods. Present work focus on
synthesis of MgO nanoparticles by Neem leaves through Green method. This method is non-toxic and eco-friendly. In this work,
the precursor materials was Mg(NO3)2 and fresh Neem leaves extract. The Neem leaves extract acting as a reducing agent in the
reaction. The particles thereby obtained were characterized by different analytical techniques. X-Ray Diffractometer (XRD) for
to calculate the average crystalline size, Particle Size Analyser for average particle size, Field Emission Scanning Electron
Microscope (FESEM) for morphological studies, UV-Visible spectroscopy (UV-Vis)for to analyse the absorption patterns,
Fourier Transform Infrared (FTIR) spectroscopy is used for analysing the functional groups which is involved in the reaction.

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access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/3.0/).

Keywords:Magnesium Oxide; Green Synthesis; Neem leaves; Seed germination

____________

* Corresponding author. Tel.: +0-984-367-0543

E-mail address: krishnakrishna1310@gmail.com

2214-7853 © 2015 Elsevier Ltd. All rights reserved.

Selection and peer-review under responsibility of the conference committee members of the International conference on Nano Science & Engineering
Applications - 2014
doi:10.1016/j.matpr.2015.10.027
 S. Krishna Moorthy et al. / Materials Today: Proceedings 2 (2015) 4360 – 4368 4361

1. Introduction

Green synthesis techniques make use of moderately pollutant free chemicals to synthesis Nanoparticles and
embrace the use of benign solvents such as water, natural extracts[1]. Green chemistry seeks to reduce pollution at
source. It is enhanced to prevent waste than to treat or clean up waste after it is formed. Though physical and
chemical methods are trendier for nanoparticles synthesis, the biogenic fabrication is a better choice due to eco-
friendliness[2]. Nanoparticles due to their smaller size and large surface to volume ratio exhibit remarkable novel
properties and methodical applications in the field of biotechnology, sensors, medical, catalysis, optical devices,
DNA labelling, drug delivery and they are rewardingly treated as a bridge between bulk material and atomic and
molecular structures[5].

MgO nanoparticles have found fabulous application in biomolecular detection, diagnostics, and
microelectronics. Green synthesis of MgO nanoparticles were agreed out using Neem leaf extract for the eco-
friendly development of novel technologies[12]. Recently, nanoparticles (NPs) have attracted a lot of attention
because of their use in a variety of areas such as electronic, cosmetic, biomedical, energy, environmental, catalytic
and material applications[16]. The large increase in the of use of NPs has stimulated researchers to know the
application of NPs in plant growth. Limited studies have been reported on both the positive and negative effects of
NPs on plants[17].

Researchers have reported both positive and negative evidences for the mechanism. Moreover, the toxicity
of NPs depends on their properties, test organism species and surrounding conditions[18]. Bulk Magnesium this
article, it is show Oxide (MgO) is very insoluble in soil; however, plant roots have the ability to solubilise MgO in
the vicinity[19]. In the increased surface-to-volume ratio of nano-MgO, which was prepared by Green Method in
our laboratory and characterised, was found very suitable for seed germination[20]. This could be observed visually
in Solanumlycopersicum and Cicer arietinum seed germination.

2. Experimental Methods

2.1 Materials and Methodology

Present investigation is focused on the synthesis of the MgONPs. The green synthesis method is used to
synthesis the MgONPs using the precursor materials such as Magnesium nitrate and Neem (Azadirachta indica) leaf
extract has been used as reducing agent to synthesis the corresponding NPs.
2.2 Preparation of Neem Leaf Extract
To prepare the Neem leaves extract; 5 g of Neem leaves were washed thoroughly with distilled water and
dried for 15-20 minutes at room temperature. The extract solution was prepared by boiling dried leaves in 500ml
beaker consist 200 ml of distilled water for one hour at 100oC .Freshly prepared Neem leaf extract was used for the
synthesis of MgONPs . Freshly prepared extracts alone have been used throughout the study.
2.3 Synthesis of MgO Nanoparticles
In the experiment, 5 ml of fresh leaves extract and 20ml of distilled water was added to a 250ml beaker and
heated at 60oC. 5 gram of Magnesium Nitrate is added to the solution and heated at 80 oC with continuous stirring for
4hours. The Magnesium nitrate ions were reduced to Magnesia or Magnesium Oxide nanoparticles by using Neem
leaves extract. The formation of Magnesium oxide nanoparticles (MgONPs) have been observed by color change of
the solution from yellow to yellowish-brown color.
3. OPTIMIZATION STUDIES FOR THE SYHNTHESIS OF MgONPs
3.1 Influence of Neem (Azadirachta indica) leaf extract
The green synthesis of MgONPs was mediated by using different concentrations of Neem leaf extracts.
Different concentration viz. 5ml, 10ml, 25ml, 50ml of freshly prepared aqueous extracts have been used as a
reducing agent. Among 5ml, 10ml, 25ml, 50ml concentrations used 5ml of extract was found to good for the
synthesis of MgONPs.
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3.2 Effect of stirrer temperature

The influence of stirring temperature for the green synthesis of MgONPs were studied by exposing the precursors in
range of temperature from 35oC to 150oC. Among 35oC, 50oC, 80oC, 100oC and 150oC Stirring temperature used
80oC of Stirring temperature was found to good for the synthesis of MgONPs.

3.3 Influence of Calcination Temperature

The Calcination temperature is used for the crystallisation purpose. The study exposed the synthesised MgONPs in
various calcinations temperature such as 300, 500 and 700oC for one hour and average size of the MgONPs have
been measured using Debye Scherer's formula (0.9λ/ (B*cosθ). Among 300oC, 500oC and 700oC calcination
temperature used 500oC of calcination temperature was found to good for the synthesized of MgONPs.
4. Result and Discussion
Magnesium Oxide was synthesized by Green synthesis method from Magnesium Nitrate Mg (NO 3)2, NaOH
using Neem (Azadirachta indica) Leaf Extract. The influence of various parameters viz. Stirring temperature,
concentration of Neem leaf extract, calcinations temperature were also checked and conditions were optimized for
the synthesis of MgONPs .
4.1 XRD and UV-Vis
A white coloured MgONPs were obtained as powder and the result of the XRD showed a little amount of
impurities and the structure was found to be cubic in nature. Debye Scherer's formula is used to find the particle size
of synthesised MgONPs (0.9λ/ (B*cosθ) and the size was found to be 25 and 27nm .UV-Vis spectroscopy shows a
specific absorption peak at 273.5 nm which is in range of 260 to 280 nm which is specific for MgONPs. The band
gap of the magnesium oxide nano particles was estimated from the UV-VIS absorption. It was observed that the
band gap of the sample constant i.e. (7.5eV) for constant calcinations temperature at 500 and 700 oC.
 S. Krishna Moorthy et al. / Materials Today: Proceedings 2 (2015) 4360 – 4368 4363

Fig.1. a. XRD pattern for the MgONPs, b. UV-Vis Spectrum of the MgONPs

4.2 FTIR and PSA

The FTIR spectrum of MgO nanoparticles is shown in Figure 2. The broad absorption peaks at 3416 cm -1
and 1615 cm-1 is due to the stretching and the bending vibration of water, respectively. The peak at 588 and
694cm−1 is assigned to the Mg–O stretching vibration in Mg (OH)2. The absorption peak at 1481 cm-1 is the
bending vibration of OH bond. Absence of 3686 cm-1 sharp peak due to antisymmetric stretching vibration in the
Mg (OH)2 crystal structure further confirms that calcinating at 500°C and 700 oC for 1hrs in air completely
transforms hexagonal structure of Mg(OH)2 to cubic MgO.The prepared Magnesium Oxide NPs were ultra-
sonicated and suspended in the ethanol solution. The sizes of the MgO NPs in the suspensions were estimated using
particle size analyser. The histograms of the particle sizes verse undersize percentages are shown in the figure and
the average particle size of the MgONPs is 43nm.
4364 S. Krishna Moorthy et al. / Materials Today: Proceedings 2 (2015) 4360 – 4368

Fig.2. a. FTIR spectra for the MgONPs, b.Average particle size of the MgONPs
4.3 FESEM and EDX
FESEM was used to study the microstructure character of the MgO nano crystals. The average size of the
MgONPs was found to be 231.1nm and they showed small amount of agglomeration. EDX pattern infers the
presence of elements Mg and O. The elemental percentages were obtained from EDX pattern. The average presence
of Mg is 46.20 and the presence of O is 53.80.

Fig.3.a. FESEM images of MgONPs and b. EDX spectra of MgONPs

 S. Krishna Moorthy et al. / Materials Today: Proceedings 2 (2015) 4360 – 4368 4365

5. Seed Germination application

Cicer arietinum (Chick pea) and Solanumlycopersicum (Tomato) seeds were immersed in 10% sodium
hypochlorite solution for 10 min to ensure the surface sterility. Followed by all the seeds were soaked in DI water
for 1 hour. After 1 hour, a few seeds were taken out and dipped in nano-MgO suspension solution. After 2 hours, a
few seeds from this solution were taken out and rinsed thoroughly with DI water and a few seeds were kept in the
MgO suspension. These seeds were then transferred onto filter paper with 10–12 seeds per Petri dish.
In total, three samples had been created:
a) Seeds in DI water only (Sample A)
b) Seeds suspended in the MgONPs suspension for 2 hours and then thoroughly rinsed with DI water (Sample B)
c) Seeds remaining suspended in MgONPs suspension (Sample C).
The Petri dishes were covered and placed in the dark for 3 days at room temperature. Almost 90% seeds were
germinated and developed roots and leaves, which were photographed of as shown in Figure 4.In this study, seeds
showing the emergence of radical out of the seed coat were recorded as being germinated. The sprouted seeds are
planted to investigate the effect of Nanoparticles on plant growth. After measuring the length of the leaves after 10
days, the leaves from sample A, sample B and sample C is taken to examine for the presence of total chlorophyll and
carotenoids content. The experiment was performed in triplicates.

5.1Estimation of total chlorophyll and carotenoid content

Extraction Process for the above three samples 0.5 grams (leaves) have been put separately in 25ml ethanol. These
samples were crushed and the supernatant is collected and characterized under UV-Visible spectroscopy for the
investigation of the total presence of chlorophyll and carotenoids[27].
Chlorophyll content of the samples were calculated using

Ca 13.95 A665  6.88 A649 (1)

Cb 24.96 A649  7.32 A665 (2)

1000 A470 – 2.05 Ca – 114.8 Cb

Cx  c (3)
245
Where, Ca – Chlorophyll a, Cb – Chlorophyll b, Cx+c – Carotenoids and A470, A649, and A665 – Absorption at 470nm,
649nm and 665nm respectively.
The calculated results are represented in the Fig. 4. (a) and (b)
4366 S. Krishna Moorthy et al. / Materials Today: Proceedings 2 (2015) 4360 – 4368

Fig.4.Pictorial Illustration of chlorophyll and carotenoids a.Cicer arietinum and b.Solanumlycopersicum

The green synthesised MgONPs were used in the study of seed germination process using Cicer arietinum
and Solanumlycopersicum. The study results revealed that the germination process was influenced by MgONPs in
Cicer arietinum not in Solanumlycopersicum. The plants emerged from the exposed seeds are also takento study the
total amount of chlorophyll and carotenoids present in Cicer arietinum and Solanumlycopersicumleaves. Cicer
arietinum showed a good quantity of chlorophyll and carotenoids content than Solanumlycopersicumwhich highly
coincides with seed germination process.

5. Summary and Conclusion

Magnesium Oxide was synthesized by Green synthesis method from Magnesium Nitrate Mg (NO 3)2 using
Neem (Azadirachta indica) Leaf Extract. The influence of various parameters viz. Stirring temperature,
concentration of Neem leaf extract and calcinations temperature were also checked and conditions were optimized
for the synthesis of MgONPs. The synthesized MgONPs are investigated by using the characterization techniques
such as XRD, UV-Vis, FTIR, FESEM and PSA to conform the presence of MgONPs.The green synthesised
MgONPs were used in the study of seed germination process using Cicer arietinum and Solanumlycopersicum. The
 S. Krishna Moorthy et al. / Materials Today: Proceedings 2 (2015) 4360 – 4368 4367

study results revealed that the germination process was influenced by MgONPs in Cicer arietinum not in
Solanumlycopersicum.

6. Acknowledgement
I express my sincere gratitude to my project guide Dr. K. Venkateswara Rao, Associate professor of
Nanotechnology, Centre for Nano Science and Technology, Institute of Science and Technology, Jawaharlal Nehru
Technological University Hyderabad, for giving invaluable guidance, support, help which made to me think and do
this research work with confidence.Foremost, I would like to express my sincere gratitude to my advisor and my
guidanceMs. P. PremasudhaAssistant Professor of the Department of Nanoscience and Technology, Bharathiar
University.

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