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Procedia Technology 24 (2016) 761 – 766

International Conference on Emerging Trends in Engineering, Science and Technology (ICETEST

- 2015)

Preparation of Zinc Oxide Nanoparticles and its Characterization

Using Scanning Electron Microscopy (SEM) and X-Ray
Diffraction(XRD)
Ananthu C Mohana, Renjanadevi Bb*
a
Department of Chemical Engineering, Govt Engineering College Trichur, Thrissur, India
b
Associate proffessor, Department of Chemical Engineering, Govt Engineering College Trichur, Thrissur, India

Abstract

Zinc oxide can be called a multifunctional material thanks to its unique physical and chemical properties. The main objective
of this paper is the preparation of zinc oxide nanoparticles using conventional methods and the preparation using surfactant. The
first part of this paper presents the different methods of preparation of Zinc oxide nanoparticles using different precursors and its
surface modification using Poly Vinyl Alcohol (PVA). The next part of this paper deals with characterization of the prepared
zinc oxide using Scanning Electron Microscopy (SEM) and X-Ray Diffraction in order to determine which method is more
feasible in terms of particle agglomeration, particle size, particle separation.

© 2016 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
© 2016 The Authors.Published by Elsevier Ltd.
Peer-review underresponsibility
Peer-review under responsibilityofofthethe organizing
organizing committee
committee of ICETEST
of ICETEST – 2015
– 2015.

Keywords: zinc oxide;preparation; surfactant

* Corresponding author. Tel.: +0-000-000-0000 ; fax: +0-000-000-0000 .

E-mail address:author@institute.xxx

2212-0173 © 2016 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Peer-review under responsibility of the organizing committee of ICETEST – 2015
doi:10.1016/j.protcy.2016.05.078
762 Ananthu C. Mohan and B. Renjanadevi / Procedia Technology 24 (2016) 761 – 766

1. Introduction

The concept of nanotechnology was introduced by Richard Feynman in 1959, when he gave a talk called “there is
plenty of room at the bottom”. In his talk he never explicitly mentioned about nanotechnology, he suggested that it
will eventually be possible to manipulate atoms and molecules precisely. The invention of the Scanning Tunneling
Microscope in 1981 and the discovery of fullerenes in 1985 are considered as the convergence of experimental
advances which leads to the emergence of nanotechnology in 1980’s. nanoscience and nanotechnology are widely
cited to be the defining technology for 21st century and nanotechnology is defined as the control and manipulation of
matter at nano dimensions. The introduction of nanotechnology resulted in development of Nano powders that can
be used for wide range of applications. Research has been made for nano-size materials in recent years because of
their unique character differing from those in the bulk state. One of the great promises that nanoparticles of metal
oxides hold in chemical applications is their remarkable ability to chemically absorb a wide variety of molecules,
especially organic molecules that are concern as environmental hazards.
In recent years zinc oxide has promoted itself as a interesting metal oxide material because of its unique physical
and chemical properties such as high chemical and mechanical stability , broad range of radiation absorption, high
catalysis activity, electro chemical coupling coefficient, non toxic nature etc. In materials science, zinc oxide is
considered as a semiconductor in group II-VI, with a broad energy band of 3.37 eV and high band energy of 60meV.
Because of its distinct properties its widely used in many fields such as rubber industry, pharmaceutical and
cosmetic industries, textile industries, electronics and electro technology industries etc . Nanometri zinc oxide can
occur in variety of structures. It can occur in one dimensional (1D), two dimensional (2D) and three dimensional
(3D) structures. One dimensional structures make up the largest group including needles, helixes, nanorods, ribbons,
belts, wires and combs. Zinc oxide can occur in two dimensional structures such as nanopellets,
nanosheet/nanoplate.[1] Examples of three dimensional structures of Zinc oxide include snowflakes, dandelion,
flower etc.In this paper the method of synthesis, characterization, surface modification is discussed. Zinc oxide can
be synthesized using many different methods including micro emulsion synthesis, spray drying, sol-gel method,
pyrolysis, controlled precipitation , RF plasma synthesis, vapour transport process etc. controlled precipitation
method was used here for the synthesis of zinc oxide nanoparticles

2. Experimental

2.1. Materials

For the preparation of zinc oxide nano particles two different precursors were used. First one is zinc sulphate
heptahydrate (M=287.49g/mol ,Sigma Aldrich), and zinc acetate (M=219.5g/mol, Merk), Poly Vinyl Alcohol (PVA)
(Sigma Aldrich)was used as the surface modificant, distilled water was used as the solvent

2.2. Sample preparation

a) Preparation using zinc sulphate as the starting material

To the aqueous solution of zinc sulphate heptahydrate sodium hydroxide was added drop wise in a molar ratio of
1:2, under vigorous stirring, and the stirring action is continued for almost 18 hours and large amount of white
precipitate was formed, this precipitate was filtered and washed with distilled water and dried using a muffle furnace
at a temperature of 100 ƕC and it is ground to fine powders and finally the powder obtained was calcined at different
temperatures such as 500ƕC,700ƕC,900 ƕC. Here the particles are calcined at different temperatures in order to obtain
just an idea about the relation connecting yield and temperature, as the calcination temperature increases the yield
decreases
 Ananthu C. Mohan and B. Renjanadevi / Procedia Technology 24 (2016) 761 – 766 763

b) Preparation using zinc acetate as the starting material

Initially 1M zinc acetate solution was stirred vigorously, and to this vigorously stirred zinc acetate, 2M sodium
hydroxide solution was added drop wise, large amount of white slurry’s were formed, and this white slurry were
continuously stirred for 18 hours, a white precipitate was formed, which was filtered and washed with distilled water
and dried using muffle furnace and it is ground to fine powders and finally calcined at 400 °C. If the temperature is
more than 400°C then the particles starts to thermally degradates and We can observe a noticeable colour change
from white to a dark ash colour

c) Preparation using Poly Vinyl Alcohol (PVA) as surfactant

To prepare zinc oxide nanoparticles 0.01% PVA solution prepared initially and 2ml PVA was added to 1M zinc
sulphate heptahydrate solution and 2M sodium hydroxide was added to it drop wise very slowly the resulting
solution is stirred for almost 18 hours. One thing should keep in mind that if the concentration of PVA is high then it
will leads to a situation in which plenty of foam will form instead of the precipitate. After 18 hours large amount of
white precipitate was formed which was filtered and washed with distilled water and dried in a muffle furnace at a
temperature of 100°C for 2 hours then it was ground to fine powders and finally calcined at 450°C

2.3. Measurements

Scanning Electron Microscopy (SEM) images of the zinc oxide nanoparticles and the epoxy nanocomposites
were obtained using a JSM-JEOL 6390 Scanning Electron Microscope. The JSM-6390 is a high performance, low
cost scanning electron microscope with a high resolution of 3nm. The customizable graphical user interface allows
the instrument to be intuitively operated. It is equipped with an auto coater for coating the samples and the coating
time is automatically adjusted by the coater and it varies according to the nature of the sample.

3. Results and Discussions

3.1. Scanning Electron Microscopy(SEM)

Fig. 1 SEM image of zinc oxide prepared using zinc sulphate as Fig.2. SEM image of zinc oxide prepared using zinc sulphate
the starting material as the starting material

Figure 1. Shows the Scanning Electron Microscope (SEM) image of the zinc oxide nanoparticles under lower
764 Ananthu C. Mohan and B. Renjanadevi / Procedia Technology 24 (2016) 761 – 766

magnification and it shows that the particles are agglomerated and complete separation is not occurred. Fig 2 shows
its SEM image at higher magnification and we can see that the particles are held together because of weak physical
forces. Here particles were formed with size in the micron range, we want particles with size in the region of at least
100nm so it concludes that zinc oxide prepared using zinc sulphate as the staring material does not produce particles
with size in the nanometre range and also the particle separation is not good and this method of preparation was
highly affected by particle agglomeration

Fig.3 SEM image of zinc of prepared using zinc acetate as the Fig.4 SEM image of zinc oxide prepared using zinc acetate as the
Starting material starting material

Fig 3. Shows the Scanning Electron Microscope (SEM) image of zinc oxide prepared using zinc acetate as the
starting material under lower magnification. Here the particles are marginally agglomerated but the particle
separation is not good enough here also we can see that the particles are held together because of weak physical
force .Fig 4. shows the SEM images of zinc oxide under higher magnification it clearly suggests that particle
separation is not good enough and also particles with size in micron range was formed so it concludes that zinc
oxide prepared using zinc acetate as the starting material does not produce particles with size in the nanometre range
and the particle agglomeration is marginal compared to the previous method

Fig.5 SEM image zinc oxide prepared using PVA as surfactant Fig.6 SEM image of zinc oxide prepared using PVA as surfactant

Fig 5.shows the Scanning Electron Microscope image of zinc oxide prepared using zinc sulphate as the starting
 Ananthu C. Mohan and B. Renjanadevi / Procedia Technology 24 (2016) 761 – 766 765

material and Poly Vinyl Alcohol as the surfactant. Here the negative impact of particle agglomeration and particle
separation was sorted out to an extend due to the introduction of Poly Vinyl Alcohol as surfactant. Here the particle
agglomeration is very less compared to the previous methods. Fig 6. Shows the SEM images at higher magnification
and we can see that particles with size less than 100nm were formed also it gave clear idea about the particle
separation, we can see that the particles are separated smoothly and not highly affected by agglomeration

3.2. X-Ray Diffraction(XRD)

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Figure 7. XRD spectrum of Nano zinc oxide prepared using PVA as surfactant

The XRD of the synthesized zinc oxide shows broad peaks at values of 31.9, 34.5, 36.3, 56.7, and 62.9 which are
typical for the zinc oxide structure. Notable line broadening of the diffraction peaks is an indication that the
synthesized materials are in nanometre range. The average particle size has been determined from full width at half
maximum (FWHM) of the diffraction peaks using Scherrer’s equation. Which is given as t = 0.9 Ȝ/(B cos ș) where
Ȝ is the wavelength of x-ray and B is the full width at half maximum. The average particle size of zinc oxide
nanoparticles has been found to be 25nm

4. Conclusions

Zinc oxide nanoparticles were successfully prepared with and without using surfactant. Poly Vinyl Alcohol (PVA)
was used as the surfactant and the prepared Nano powder was characterized using Scanning Electron Microscopy
(SEM) And X-Ray Diffraction (XRD). According to the characterization results it’s clear that the conventional
method of preparation i.e. without any surfactant highly affected by particle agglomeration and also the particle
separation is not good enough. But when prepared using a surfactant the particle agglomeration is very less and also
the particle separation is good. And the most important thing is that the particle size of zinc oxide prepared using
PVA is in the nanometre range whereas in conventional method of preparation particle size in the micron range.
According to the XRD characterization the average particle size of zinc oxide prepared using PVA as surfactant has
been determined using scherrer’s equation. The average particle size of zinc oxide nanoparticles has been found to
be 25nm

References

[1] Agnieszka Kołodziejczak-Radzimska and Teofil Jesionowski(2014) “ Zinc Oxide—From Synthesis to Application: A Review” materials
2833-2881
766 Ananthu C. Mohan and B. Renjanadevi / Procedia Technology 24 (2016) 761 – 766

[2] AbdulazizBagabas, Ahmad Alshammari, Mohamed FA Aboud and Hendrik Kosslick(2013) ”Room-temperature synthesis of zinc oxide
nanoparticles in different media and their application in cyanide photo degradation” Nanoscale research letters

[3] Hong, R.; Pan, T.; Qian, J.; Li, H.(2006) “Synthesis and surface modification of ZnO nanoparticles”. Chem. Eng. J. ,119, 71–81.

[4] Ristiü, M.; Musiü, S.; Ivanda, M.; Popoviü,S (2005) . “Sol–gel synthesis and characterization of nanocrystallineZnO powders”. J. Alloy.
Compd., 39, L1–L4.

[5] Ismail, A.A.; El-Midany, A.; Abdel-Aal, E.A.; El-Shall, H. (2005) “Application of statistical design to optimize the preparation of ZnO
nanoparticles via hydrothermal technique”. Mater. Lett. 59, 1924௅1928.

[6] Singhal, M.; Chhabra, V.; Kang, P.; Shah, D.O.(1997). “Synthesis of ZnO nanoparticles for varistor application using Zn-substituted Aerosol
OT microemulsion”. Mater. Res. Bull., 32, 239௅247.

[7] A.Matei, I. Cernica1, O. Cadar, C. Roman, V. Schiopu1. “Synthesis and characterization of ZnO – polymer nanocomposites”