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International Journal of Mechanical Engineering and Technology (IJMET)

Volume 6, Issue 8, Aug 2015, pp. 139-143, Article ID: IJMET_06_08_013


Available online at
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ISSN Print: 0976-6340 and ISSN Online: 0976-6359
IAEME Publication
________________________________________________________________________

MORPHOLOGICAL CHARACTERISATION
OF POLY METHYL METHACRYLATE FOR
SURFACE COATING OF METALS
N. Jayakumar
Ph.D research scholar, Department of Mechanical Engineering,
AMET University, Chennai, India
Dr. S. Mohanamurugan
Professor and Head, Department of Automobile Engineering,
Saveetha University, Chennai, India
Dr. R. Rajavel
Professor and Head, Department of Mechanical Engineering,
AMET University, Chennai, India
V. Srinivasan
Assistant Professor, Department of Mechanical Engineering,
Bharath University, Chennai, India
ABSTRACT
Poly methyl methacrylate (PMMA) is one of the most important industrial
plastics. On the whole, characterization of PMMA refers to the general
process by which its structure and properties are investigated and measured.
It is a radical process, without which no scientific understanding of PMMA
can be made certain. The scope of the term characterization of PMMA
differs. Some researchers limit its use to modi operandi which study the
microscopic configuration and chattels of PMMA which is called microscopy
while others use it to refer to any analysis process including macroscopic
techniques viz. mechanical testing, thermal study and density computation.
Here, we are adopting both macroscopic techniques as well as microscopic
techniques such as Fourier transform infrared spectroscopy (FTIR) and X-Ray
diffraction (XRD) tests to characterize PMMA in order to verify whether the
material is pure and amorphous in nature so that this material could be used
subsequently for metal coating.
Key words : Characterization, Poly methyl methacrylate, X-Ray diffraction
and Fourier transform infrared spectroscopy.

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N. Jayakumar, Dr. S. Mohanamurugan, Dr. R. Rajavel and V. Srinivasan

Cite this Article: Jayakumar, N., Dr. Mohanamurugan, S., Dr. Rajavel, R. and
Srinivasan, V. Morphological Characterisation of Poly Methyl Methacrylate
for Surface Coating of Metals. International Journal of Mechanical
Engineering and Technology, 6(8), 2015, pp. 139-143.
http://www.iaeme.com/IJMET/issues.asp?JTypeIJMET&VType=6&IType=8

1. INTRODUCTION
The first step in characterization of PMMA is a macroscopic observation. It means,
simply looking at the material with naked eye. This simple process could yield a large
amount of information about the material such as the color of the resin, its luster, its
shape ie whether it exhibits regular form or crystalline form, its composition ie is it
made up of different phases?, its structural features ie does it contain porosity? etc.
The next step is the microscopic observation that includes FTIR and XRD tests.
Juan Li studied the chemical structure of the PMMA, PMMA-b-PDMAEMA and
PMMA-b-PDMAEA polymers by FT-IR spectroscopy on a Nicolet 6700 FT-IR
spectrophotometer (Thermo Inc., America) with the polymer samples dispersed in
KBr pellets. The copolymer compositions were determined by NMR spectroscopy.
HNMR measurements were performed on a UNITY-plus 400 M nuclear magnetic
resonance spectrometer(Varian, Inc., America) using CDCl as the solvent. XRD was
used to test the crystalline of the polymers on XPERT PRO X-ray diffraction
(PANalytical, Netherlands). [1]
Shahzada Ahmad illustrated the diffractograms of PMMA and PMMASiO2
composites in the 2 range between 5 and 90 degree, which were s imilar and without
any sharp diffraction peaks confirming their non-crystalline nature. The interlayer
spacing of the system was determined by the diffraction peak in the X-ray method,
using the Bragg equation = 2dsin , where d is the spacing between diffractional
lattice planes, is the diffraction position while is the wavelength of the X-ray
(15405 ). PMMA is known to be an amorphous polymer and showed three broad
peaks at 2 values of 12, 30 and 32 (d spacing around 7 , 294 and 279 ),
with their intensity decreasing systematically. The shape of the first most intense peak
reflects the ordered packing of polymer chains while the second peak denotes the
ordering inside the main chains. The addition of SiO2 does not induce any
crystallinity in these polymers. This also explains the homogeneous nature of these
samples. He also depicted that the FTIR spectra of PMMA, PMMASiO2 and
PMMATiO2were similar except for a few changes in the spectra of the nano
composites. The features that were similar identified the presence of PMMA in all of
them. [2]
A.K.Tomar characterized the structure of PAni powder, pure PMMA and their
blended films by using X-ray Diffraction (XRD) and Fourier Transform Infrared
spectroscopic (FTIR) techniques.
In his characterization, X-ray diffraction patterns of unblended PMMA and
various PMMA-PAni blended films were presented and it was apparent that X-ray
pattern of PMMA matrix could show broad bands peaking at around 2= 15.45,
29.93 and 41.22 indicating its amorphous nature. The X-ray pattern of various PAniPMMA blended films showed the absence of the peaks which were present in PAni
with the broadening of peak of PMMA indicating the amorphous nature of PAniPMMA blended films. The structure of pure PMMA was primarily characterized by
the 1736 cm band assigned to free lateral C=O stretching in the FTIR study. [3]

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Morphological Characterisation of Poly Methyl Methacrylate for Surface Coating of Metals

S. Sathish adopted FTIR and XRD analysis for characterizing a thin film of
PMMA. In FTIR spectroscopy, the bands at about 677 cm- and 750 cm- were
assigned to out of plane OH bending. The band at around 980 cm- was the
characteristic absorption vibration of PMMA. The bands at about 1060 cm-, 1245 cm, 1730 cm- and 2926 cm- were assigned to (C-O) stretching vibration, wagging
vibration of C-H, C=O stretching and C-H stretching respectively. The relatively
broad and intense absorption observed at around 3400 cm- indicated the presence of
O-H stretching vibration. It was also found that both as grown and annealed films
showed similar FTIR spectrum which eliminated the presence of any impurity in
PMMA thin films. The X-ray diffraction indicated amorphous nature with large
diffraction maximum that decreases at large diffraction angles. The observed broad
humps in the XRD spectrum indicated the presence of crystallites of very low
dimensions. The absence of any prominent peaks indicated the amorphous nature of
the thin PMMA films. [4]
Devikala experimented XRD, SEM and techniques to characterize PMMAZirconium dioxide composite. The XRD patterns of polymers and polymer
composites were recorded using Philips XPERT PRO diffractometer with Cu K (=
1.54060 ) incident radiation. The XRD pattern for PMMA showed peaks at 2 is
equal to 14.50, 22.49, 29.45 and 41.41 and relative intensities obtained for the
polymer matched with the JCPDS Card no. 13-0835 file, identifying it as PMMA. The
average crystallite size of PMMA was determined using XPert High Score plus
software and it was found to be 0.1344 m. From XRD of composites, she could say
that the crystallinity of PMMA had decreased considerably upon the addition of
ZrO2. [5] The average crystallite size was found to be 0.1413 m. [6]

2. EXPERIMENTAL DETAILS
2.1. Material
White, crystalline PMMA powder with melting point > 150C, molecular weight 450550K and size 120-160 mesh was obtained from Alfa Aesar (Product Number 43982)
through H.Chandanmal & Co., Chennai, India.

2.2. Characterization
To comprehend the properties of the polymer material, it becomes necessary to know
the features of its structure. X-Ray Diffraction technique (XRD) and Fourier
Transform Infrared Spectroscopy (FTIR) technique were employed to characterize
PMMA.

2.3. XRD Analysis


X-ray diffraction is one of the most important characterization tools used in materials
science to determine the size and the shape of the unit cell for any compound most
easily. X-ray diffraction provides the most definitive structural information such as
inter atomic distances and bond angles. Table 1 shows the measurement conditions
for the XRD test conducted for the PMMA powder.

2.4. FTIR Test


FTIR spectroscopy is the most preferred method of infrared spectroscopy. In this
spectroscopy, infrared radiation was passed through the sample PMMA powder.
Some of the infrared radiation was absorbed by the sample, some of it was reflected
and some of it was transmitted. The resulting spectrum represented the molecular
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N. Jayakumar, Dr. S. Mohanamurugan, Dr. R. Rajavel and V. Srinivasan

absorption, reflection and transmission, creating a molecular fingerprint of the


sample. Like a fingerprint no two unique molecular structures produce the same
infrared spectrum. This infrared spectroscopy is also useful for several types of
analysis such as identifying material, determining the quality or consistency of the
sample and determining the amount of components in a sample.
Table 1 Measurement conditions for XRD test
X-Ray

Scan speed/Duration
time

30kV,100mA

3.0000 deg/min

Goniometer
Attachment

Smart Lab
Standard

Step width
Scan axis

Filter
CBO selection list
Diffracted beam
mono
Detector

Cu_K-beta
BB

Scan range
Incident slit

0.0200 deg
Theta/2-Theta
10.0000-90.0000
deg
2/3 deg

None
SC-70
CONTINUOU
S

Length limiting slit


Receiving slit # 1

10.0 mm
2/3 deg

Receiving slit # 2

0.300 mm

Scan mode

3. RESULTS AND DISCUSSION

intensity (cps)

In order to collect information about the structure, XRD and FTIR spectra of PMMA
powder were examined. The morphology of pure PMMA powder was studied by an
XRD test. The X-ray diffraction pattern of PMMA is presented in Figure 1. From the
figure, it is obvious that X-ray pattern of PMMA shows broad bands peaking at
around 2= 13.85, 30.09 and 42.06. The X-ray pattern, peaking around these
angles indicates the amorphous nature of the PMMA powder.
3500
3000
2500
2000
1500
1000
500
0
10

20

30

40

50

60

70

80

90

2- theta (deg)

Figure 1 XRD pattern of pure PMMA powder

The FTIR spectra of pure PMMA powder are presented in Figure 2, with peaks at
1185 cm- (Transmission) 1756 cm- (Reflection) 1783 cm- (Absorbance). These
peaks confirm the absence of any additional bands other than those of PMMA and
further they remain unperturbed in all the three spectra which indicate the purity of
the polymer tested.

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Morphological Characterisation of Poly Methyl Methacrylate for Surface Coating of Metals

100

100

0.6

80
80

0.4

%T

%R

60

Abs

60

0.2

40
40
4000

3000
2000
Wavenumber [cm-1]

1000

400

20
4000

3000
2000
Wavenumber [cm-1]

1000

0
400 4000

3000
2000
Wavenumber [cm-1]

1000

Figure 2 FTIR spectra of PMMA powder for Transmission, Reflection and Absorbption

4. CONCLUSION
The amorphous nature of PMMA was confirmed through the XRD test result. Due to
the intertwining chains, amorphous polymers experience viscous flow when heated.
They also have a decreased chance of warping and shrinking during molding, casting
or coating than semi-crystalline plastics. The amorphous nature of PMMA may also
exhibit rubber- like properties, able to stretch and deform without fracturing. All these
features of PMMA make it one of the best materials for metal coating.
The FTIR analysis showed that there are no impurities in the PMMA powder.
Impurities in a virgin polymer ruin the possibilities of using the material for certain
applications that include using it as a coating material. As the FTIR analysis showed
the absence of impurities, it was ascertained that PMMA could subsequently be used
to coat metal surfaces.

5. REFERENCES
[1]

[2]

[3]

[4]

[5]

[6]

Li, J., Jiang, T.-T., Shen, J.-N. and Ruan, H.-M. Preparation and Characterization
of PMMA and its Derivative via RAFT Technique in the Presence of Disulfide as
a Source of Chain Transfer Agent. Journal of Membrane and Separation
Technology, 1(2), 2012.
Ahmad, S., Ahmad, S. and Agnihotry, S. A. Synthesis and characterization of in
situ prepared poly (methyl methacrylate) nanocomposites. Bull. Mater. Sci.,
30(1), February 2007, pp. 3135. Indian Academy of Sciences.
Tomar, A. K., Mahendia, S. and Kumar, S. Structural characterization of PMMA
blended with chemically synthesized PAni. Adv. Appl. Sci. Res., 2(3), 2011, pp.
327-33.
Sathish, S. and Chandar Shekar, B. Preparation and Characterization of nano
scale thin PMMA films. Indian Journal of Pure and & Applied Physics, 52,
January 2014, pp 64-67.
Kuruvinashetti, M., Ismail, M. and Suresha, B. Morphological Two-Body
Abrasive Wear Behavior of Short Glass Fiber and Particulate Filled Polymethyl
Methacrylate Composites. International Journal of Mechanical Engineering and
Technology, 5(9), 2014, pp. 86-90.
Devikala, S., Kamaraj, P. and Arthanareeswari, M. Preparation, Characterization
and Anticorrosive Properties of a Novel PMMA/ ZrO Composite. Indian
Journal of Applied Research, 4(5), May 2014, ISSN-2249-555X.

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