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 Thermal and Rheological
Measurement Techniques for
Nanomaterials Characterization
Volume 3
Edited by
Sabu Thomas
Raju Thomas
Ajesh K. Zachariah

Raghvendra Kumar Mishra

Elsevier
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The Boulevard, Langford Lane, Kidlington, Oxford OX5 1GB, United Kingdom
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Publisher (other than as may be noted herein).
Notices
Knowledge and best practice in this field are constantly changing. As new research and
experience broaden our understanding, changes in research methods, professional practices,
or medical treatment may become necessary.
Practitioners and researchers may always rely on their own experience and knowledge in
evaluating and using any information, methods, compounds, or experiments described herein.
In using such information or methods they should be mindful of their own safety and the safety
of others, including parties for whom they have a professional responsibility.
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List of Contributors
Jiji Abraham
Mahatma Gandhi University, Kottayam, India
Elaheh Allahyari
Mahatma Gandhi University, Kottayam, India; Islamic Azad University, Tehran, Iran
Gudimamilla Apparao
Acharya Nagarjuna University, Guntur, India
Jayesh Cherusseri
Mahatma Gandhi University, Kottayam, India
Cintil Jose Chirayil
Newman College, Thodupuzha, India
Soney C. George
Amal Jyothi College of Engineering, Kottayam, India
Gurram Giridhar
Acharya Nagarjuna University, Guntur, India
Jose James
St. Joseph’s College, Moolamattom, India
Karingamanna Jayanarayanan
Amrita Vishwa Vidyapeetham, Amrita University, Coimbatore, India
Nandakumar Kalarikkal
Mahatma Gandhi University, Kottayam, India
Obey Koshy
Mahatma Gandhi University, Kottayam, India
Sravanthi Loganathan
Mahatma Gandhi University, Kottayam, India
R.K.N.R. Manepalli
The Hindu College, Machilipatnam, India
Raghvendra Kumar Mishra
Mahatma Gandhi University, Kottayam, India; Indian Institute of Space Science and
Technology, Thiruvananthapuram, India
Oluwatobi S. Oluwafemi
University of Johannesburg, Johannesburg, South Africa
G. Pugazhenthi
Indian Institute of Technology Guwahati, Guwahati, India
Nanoth Rasana
Amrita Vishwa Vidyapeetham, Amrita University, Coimbatore, India

xi
xii List of Contributors

El Hadji Mamour Sakho

Mahatma Gandhi University, Kottayam, India
Ashin Shaji
Mahatma Gandhi University, Kottayam, India
Lakshmanan Subramanian
Amrita Vishwa Vidyapeetham, Amrita University, Kollam, India
Sabu Thomas
Mahatma Gandhi University, Kottayam, India
Ravi Babu Valapa
Centre for Biopolymer Science and Technology, A Unit of Central Institute of Plastics
Engineering and Technology (CIPET), Kochi, India
Ajesh K. Zachariah
Mar Thoma College, Tiruvalla, India
Editor Biographies
Professor (Dr.) Sabu Thomas is the Director of International and
Interuniversity Center for Nanoscience and Nanotechnology, Mahatma
Gandhi University, Kottayam, Kerala, India. He is also a full professor of
Polymer Science and Engineering and School of Chemical Science of the
same University. He is a fellow of many professional bodies. Professor
Thomas has co-authored many papers in international peer-reviewed
journals in the area of polymer processing. He has organized several
international conferences. Professor Thomas’s research group is in
specialized areas of polymers, which includes polymer blends, fiber-filled
polymer composites, particulate-filled polymer composites and their
morphological characterization, aging, and degradation, pervaporation
phenomena, sorption, and diffusion, interpenetrating polymer systems,
recyclability and reuse of waste plastics and rubbers, elastomeric cross-
linking, and dual porous nanocomposite scaffolds for tissue engineering.
Professor Thomas’s research group has extensive exchange programs with
different industries, research, and academic institutions all over the world
and is performing world-class collaborative research in various fields. The
Professor’s Center is equipped with various sophisticated instruments and
has established state-of-the-art experimental facilities which cater to the
needs of researchers within the country and abroad. He has more than 700
publications, 50 books, H Index-78 and 3 patents to his credit. He is a
reviewer to many international journals. Professor Thomas has attained
5th Position in the list of Most Productive Researchers in India in 2008e16.

Professor (Dr.) Raju Thomas is currently Vice Chancellor of Middle East

University FZE, Al Hamra, Ras Al Khaimah, United Arab Emirates.
Dr. Thomas started his Professorship from the Research and Postgraduate
Department of Chemistry, Mar Thoma College, Thiruvalla-3, Kerala,
India. Dr. Thomas procured his PhD under the supervision of Professor
(Dr.) Sabu Thomas, Director of International and Interuniversity Center
for Nanoscience and Nanotechnology, Mahatma Gandhi University,
Kottayam, Kerala, India. He has extensive research experience in
Nanoscience and Nanotechnology. He has 12 years of research experience
in the Organic Chemistry and Polymer Chemistry laboratories of the
School of Chemical Sciences, Mahatma Gandhi University, Kottayam,
Kerala, India. He has also worked in the laboratory of Applied Rheology
and Polymer processing of Katholieke University, Leuven, Belgium, and
in the laboratory at Leibniz Institute of Polymer Research, Dresden,

xiii
xiv Editor Biographies

Germany. He has widely studied the kinetics of curing, morphology

development, and structural characteristics of in situ-cured
nanocomposites based on epoxy resin and reactive rubbers. His research is
reflected in his six published research articles in international journals, and
additional articles which are currently under review. In addition, many
articles have been published in popular journals. He has co-authored many
chapters and is co-editor of a book entitled Micro and Nanostructured
Epoxy/Rubber Blends which was recently published by Wiley and Sons.
He has attended many national and international seminars/conferences and
presented many research papers. He is an approved research guide in
Chemistry at Mahatma Gandhi University, Kottayam, India and has
availed projects from University Grants Commission (UGC), Department
of Science and TechnologyeScience and Engineering Research Board
(DSTeSERB) and Kerala Science Council for Science, Technology, and
Environment (KSCSTE).

Dr. Ajesh K. Zachariah is working as Assistant Professor in the

Department of Chemistry, Mar Thoma College, Kerala, India. He has
many publications in the field of materials chemistry, and polymer
nanocomposites and has one national patent. He is an expert in
sophisticated techniques such as Atomic Force Microscopy (AFM), X-ray
diffraction Technique (XRD), Gas Permeability Tester, and Dynamic
Mechanical Analyzer (DMA). He has many years’ experience in the field
of nanoscience and nanotechnology.

Raghvendra Kumar Mishra is currently working as Senior Research

Fellow at the International and Interuniversity Center for Nanoscience and
Nanotechnology, Mahatma Gandhi University, India. He has received
India’s most prestigious Visvesvaraya Research Fellowship, and he is
currently serving as Visvesvaraya Fellow. He has widely studied the
processing of blends, in situ generation micro- and nanofibrillar
composites, electromagnetic shielding effect of nanocomposites,
decorating and alignment of carbon nanotubes, and thermal, dynamic
mechanical, and structural relationships in polymer blends and
nanocomposites. He has won several awards from different organizations
and technology events. He is serving as reviewer in many international
journals, for example, Environmental Chemistry Letters (Springer). He has
research experience in Mechanical Engineering, Materials Science and
Technology, and Nanoscience and Nanotechnology. His areas of research
are multidisciplinary, which include thermodynamics, heat transfer,
refrigeration and air-conditioning, fluid mechanics, machine design, solid
mechanics, machine theory, power plant engineering, metal and ceramic
 Editor Biographies xv

processing. In addition, he specializes in polymers, which include polymer

recycling, polymer blends, fiber-filled polymer composites, particulate-
filled polymer composites and their morphological characterization, aging
and degradation, nanomaterials e.g., metallic, metallic oxide, carbon
nanotubes, graphene, conducting polymer blends, composites and
nanocomposites, biodegradable polymer blends and composites. He has
expertise in sophisticated characterization techniques such as dynamic
mechanical analyzer, differential scanning calorimetry, thermogravimetric
analysis, spectroscopy, vector network analyzer, scanning electron
microcopy, and atomic force microscopy (AFM).
 Instrumental Techniques for the
Chapter
1
Characterization of Nanoparticles
Cintil Jose Chirayil1, Jiji Abraham2, Raghvendra Kumar Mishra2,
Soney C. George3 and Sabu Thomas2
1
Newman College, Thodupuzha, India; 2Mahatma Gandhi University, Kottayam, India; 3Amal Jyothi College
of Engineering, Kottayam, India

CHAPTER OUTLINE
1.1 Nanotechnology and Nanomaterials 2
1.2 Classification of Nanomaterials 3
1.3 Advantages and Disadvantages of Nanomaterials 4
1.4 Opportunities Presented by Nanomaterials 5
1.5 Characterization Techniques of Nanomaterials 5
1.5.1 Optical (Imaging) Characterization Techniques 6
1.5.1.1 Confocal Laser-Scanning Microscopy 6
1.5.1.2 Scanning Near-Field Optical Microscopy 8
1.5.1.3 Two-Photon Fluorescence Microscopy 10
1.5.1.4 Dynamic Light Scattering 10
1.5.1.5 Brewster Angle Microscopy 11
1.5.2 Electron Probe Characterization Techniques 13
1.5.2.1 Scanning Probe Electron Microscopy 13
1.5.2.2 Electron Probe Microanalysis 14
1.5.2.3 Transmission Electron Microscopy 15
1.5.2.4 Scanning Transmission Electron Microscopy 17
1.5.3 Photon Probe Characterization Techniques 18
1.5.3.1 Photoelectron Spectroscopy 18
1.5.3.2 UVeVisible Spectroscopy 19
1.5.3.3 Atomic Absorption Spectroscopy 20
1.5.3.4 Inductively Coupled Plasma Spectroscopy 20
1.5.3.5 Fluorescence Spectroscopy 20
1.5.3.6 Localized Surface Plasmon Resonance 21
1.5.4 Ion Particle Probe Characterization Techniques 22
1.5.4.1 Rutherford Backscattering 22
1.5.4.2 Small-Angle Scattering 22

Thermal and Rheological Measurement Techniques for Nanomaterials Characterization. http://dx.doi.org/10.1016/B978-0-323-46139-9.00001-3

Copyright © 2017 Elsevier Inc. All rights reserved. 1
2 CHAPTER 1 Instrumental Techniques for the Characterization of Nanoparticles

1.5.4.3 Nuclear Reaction Analysis 23

1.5.4.4 Raman Spectroscopy 24
1.5.4.5 X-Ray Diffraction 25
1.5.4.6 Cathodoluminescence 26
1.5.4.7 Nuclear Magnetic Resonance Spectroscopy 27
1.5.4.8 Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass
Spectrometry 28
1.5.5 Thermodynamic Characterization Techniques 29
1.5.5.1 Thermogravimetric Analysis 29
1.5.5.2 Differential Thermal Analysis 29
1.5.5.3 Evolved Gas Analysis 30
1.5.5.4 Differential Scanning Calorimetry 30
1.5.5.5 Nanocalorimetry 30
1.5.5.6 BrunauereEmmetteTeller Method 31
1.5.6 Other Important Techniques 31
1.5.6.1 Nanoparticle Tracking Analysis 31
1.5.6.2 Tilted Laser Microscopy 31
1.5.6.3 Turbidimetry 31
1.5.6.4 Field-Flow Fractionation 32
1.5.6.5 Size-Exclusion Chromatography 32
1.5.6.6 Hydrophobic Interaction Chromatography 32
1.5.6.7 z Potential Measurements 34
1.6 Conclusions 34
Acknowledgment 34
References 34

1.1 NANOTECHNOLOGY AND NANOMATERIALS

Nanotechnology is the art and science of handling matter at the nanoscale
(down to 1/10,000,000 the width of a human hair) to create new and unique
materials and products with properties that differ significantly from those on
a larger scale [1]. Early developments in nanotechnology were initiated by
Nobel Laureate Richard Feynman, who introduced the idea of molecular ma-
chines in 1959. The importance of nanotechnology comes from the
tunability of material properties by assembling such materials at the nano-
scale level. Norio Taniguchi’s 1974 paper is the first scientific publication
in which the term “nanotechnology” was used [2]. Now nanotechnology
can be identified as the driving force behind the industrial revolution. Owing
to its enormous potential to change society, both public and private sectors
are spending a lot of money on this new technology. At the same time, sci-
entists have anxieties about the adverse effects of the basic building blocks
of nanotechnologiesdparticles smaller than one-billionth of a meterdon
health and the environment. By using nanotechnology we can design,
 1.2 Classification of Nanomaterials 3

characterize, produce, and apply nanostructures, nanodevices, and nanosys-

tems by controlling shape and size at the nanometer scale. A nanometer is
one-billionth of a meter. The difference in the properties of materials at
nanoscale compared to bulk is due to two main reasons. First is the increased
chemical reactivity of nanomaterials due to their large surface area compared
to bulk. The second is the quantum confinement effect. A nanomaterial is an
object that has at least one dimension on the nanometer scale (approximately
1e100 nm). There are several ways to classify nanomaterials based on their
origin, dimensions, and structural configuration.

1.2 CLASSIFICATION OF NANOMATERIALS

According to their origin nanomaterials are classified as follows:
1. Natural nanomaterials
Natural nanomaterials belong to the natural nanoworld and originate
from animals or minerals without any human modification or
processing. Some important examples of natural nanomaterials
include inorganic natural nanomaterials (minerals, clays, etc.),
natural carbon nanoparticles (diamond and graphite), nanoparticles
from space, nanomaterials from the animal and plant kingdoms
(cotton, collagen, bacterial fibers, exoskeleton, and endoskeleton),
and nanomaterials in insects (chitin, sponge fibers) [3].
2. Artificial nanomaterials
These are fabricated by experimental and well-defined mechanical
and fabrication processes. Examples include carbon nanotubes,
graphene, metal oxides, quantum dots, etc.
According to their number of dimensions, which are not confined to the
nanoscale range (<100 nm), nanomaterials are classified as follows:
n Zero-dimensional
For this kind of material all the dimensions measured are within the
nanosize range. The most common demonstration of zero-
dimensional nanomaterials is nanoparticles. They are amorphous or
crystalline, single crystalline or polycrystalline; composed of single
or multiple chemical elements; exist individually or incorporated in a
matrix; exhibit various shapes and forms; and can be metallic,
ceramic, or polymeric.
n One-dimensional
For these materials one dimension is outside the nanoscale, which
leads to needle-like-shaped nanomaterials. One-dimensional
materials include nanotubes, nanorods, and nanowires.
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4 CHAPTER 1 Instrumental Techniques for the Characterization of Nanoparticles

n Two-dimensional
Two of the dimensions are not confined to the nanoscale in two-
dimensional materials and they exhibit a plate-like geometry. Two-
dimensional nanomaterials include nanofilms, nanolayers, and
nanocoatings. Thickness is in the nanometer range.
n Three-dimensional
Bulk nanomaterials are materials that are not confined to the
nanoscale in any dimension. These materials are thus characterized
by having three arbitrary dimensions above 100 nm. Three-
dimensional nanomaterials can contain dispersions of
nanoparticles, bundles of nanowires, and nanotubes as well as
multiple nanolayers.
According to their structural configuration nanomaterials can be classified
into four types:
1. Carbon-Based Nanomaterials
Carbon-based materials have captured broad interest in the materials
science community for decades because of the versatility and
extremely low weight of carbon. Examples include carbon
nanotubes, graphene, fullerenes, etc. [4].
2. Metal-Based Materials
The main component of these materials is metal. Examples include
nanoplatinum, nanogold, nanosilver, metal oxides, quantum dots,
etc. [5].
3. Dendrimers
Dendrimers are nanosized, radially symmetric molecules with a well-
defined, homogeneous, and monodispersed structure that has a
typically symmetric core, an inner shell, and an outer shell [6].
4. Composites
Nanocomposites are multiphase solid materials in which at least one
phase is in the nano range. Composites are of three types, namely,
ceramic matrix nanocomposite, metal matrix nanocomposite, and
polymer matrix nanocomposite.

1.3 ADVANTAGES AND DISADVANTAGES OF

NANOMATERIALS
n Advantages
o small size
o high surface area
o easy to suspend in liquids
o deep access to cells
 1.5 Characterization Techniques of Nanomaterials 5

o tunable/tailorable physical, chemical, and mechanical properties

due to extremely small size (1e100 nm)
o high strength, toughness, and ductility
o reduced energy costs
o enhanced activity (extremely large specific surface area), surface-
dependent material properties
n Challenges
o The main challenges are to develop instruments to assess exposure
to engineered nanomaterials in the air and water.
o The second challenge is to develop and validate methods to eval-
uate the toxicity of engineered nanomaterials by 2020e2030.
o The last challenge is to develop tools to properly assess risks to
human health and to the environment.

1.4 OPPORTUNITIES PRESENTED BY

NANOMATERIALS
Now, nanotechnology is described as a revolutionary discipline because of
its possible impression on industrial applications. Through the use of
emerging nano techniques, nanotechnology can offer possible remedies to
many problems. Because nanotechnology is an interdisciplinary area there
are many research fields and several potential applications that involve
nanotechnology. Because nanomaterials possess unique, beneficial phys-
ical, chemical, and mechanical properties, they can be used for a wide va-
riety of applications. Fig. 1.1 shows some key applications of nanomaterials.

1.5 CHARACTERIZATION TECHNIQUES OF

NANOMATERIALS
Nanomaterials commonly consist of at least two of the following units:
metallic, semiconducting, and organic particles or molecules. Additionally,
nanomaterials are generally coated with polymers or biorecognition mole-
cules to improve biocompatibility and selective targeting of biologic mole-
cules. A common feature of all nanomaterials is their large ratio of surface
area to volume, which may be orders of magnitude greater than that of
macroscopic materials. Still, the final size and structure of nanomaterials
depend on the salt and surfactant additives, reactant concentrations, reaction
temperatures, and solvent conditions used during their synthesis. Thus, the
comprehension of these physicochemical properties as well as the funda-
mentals of the associated measuring methods is necessary before character-
izing nanomaterials and developing reproducible synthesis procedures to
optimize the medical application of nanomaterials.
6 CHAPTER 1 Instrumental Techniques for the Characterization of Nanoparticles

n FIGURE 1.1 Potential applications of nanomaterials.

Characterization refers to the study of a material’s features such as its

composition, structure, and various properties such as physical, chemical,
electrical, magnetic, etc. There are plenty of techniques available on the
market that were initially used for colloidal particles (e.g., microscopy,
spectroscopy, and magnetic resonance), but each of these techniques has
a certain degree of uncertainty. Particle size distribution (PSD) plays a
fundamental role in controlling the properties of different nanomaterials.
For example, the chemical reactivity of nanomaterials, which mostly differs
from that of macroscale or microscale materials, is usually affected by the
nanoparticle (NP) surface/volume ratio. Particle size also determines NP
diffusivity and the ability of NPs to permeate cell membranes. PSD analysis
thus allows monitoring of NP aggregation or release of NP-surface modi-
fiers. There are plenty of techniques available in the literature covering spe-
cific ranges of NP size distribution, as shown in Fig. 1.2 [7].

1.5.1 Optical (Imaging) Characterization Techniques

1.5.1.1 Confocal Laser-Scanning Microscopy
Confocal microscopy, most frequently confocal laser scanning microscopy
(CLSM), is a powerful technique to produce sharp images of a sample that
would otherwise appear blurred when viewed under a conventional micro-
scope. Reconstruction of three-dimensional structures from images obtained
by this technique is possible by taking a large number of images at different
depths (a process known as optical sectioning) within a thick object.
 1.5 Characterization Techniques of Nanomaterials 7

n FIGURE 1.2 Performance of various particle size measurement techniques (note: only a few techniques can measure particles in the nanoscale region) [7].
AFM, atomic force microscopy; NP, nanoparticle; SEM, scanning electron microscopy; TEM, transmission electron microscopy.

Scanning by one or more focused beams of light, usually from a laser or

arc-discharge source, across the specimen is used to obtain images by
confocal microscopy. An objective lens is used to focus the light beam
on the specimen and then the object is scanned using some form of scanning
device under computer control. The sequences of points of light from the
specimen are detected by a photomultiplier tube (PMT) and the output
from the PMT is built into an image and displayed by the computer [8].
n Advantages
o The ability to serially produce thin (0.5e1.5 mm) optical sections
through fluorescent specimens that have a thickness ranging up to
50 mm or more
o The ability to control depth of field
o The ability to isolate and collect a plane of focus from the sample,
thus eliminating the out-of-focus “haze” normally seen with a fluo-
rescent sample
8 CHAPTER 1 Instrumental Techniques for the Characterization of Nanoparticles

o Elimination or reduction of background information away from the

focal plane
o The ability to compensate for autofluorescence
o Minimum specimen preparation and instrument reconfiguration
n Disadvantage
o A disadvantage of CLSM is colocalization of fluorophores in the
confocal microscopedtwo or more fluorescence emission signals
can often overlap in digital images recorded by confocal
microscopy because of their close proximity within the specimen
n Applications
o This technique has gained popularity in the scientific and
industrial communities and typical applications are in life
sciences, semiconductor inspection, and materials science. It is
widely used in numerous biological science disciplines, from cell
biology and genetics to microbiology and developmental biology.
It is also used in quantum optics and nanocrystal imaging and
spectroscopy [9].

1.5.1.2 Scanning Near-Field Optical Microscopy

Scanning near-field optical microscopy (SNOM) gives simultaneous mea-
surements of topography and optical properties (fluorescence) and provides
a direct correlation between surface nano features and optical/electronic
properties. SNOM is based on scanning with an arbitrarily small aperture,
which is illuminated from the back side at a close but constant distance,
across a sample surface and recording optical information pixel by pixel,
collecting transmitted, reflected, or fluorescent light to form an image. In
SNOM, the excitation laser light is focused through an aperture with a
diameter smaller than the excitation wavelength, resulting in an evanescent
field (or near field) on the far side of the aperture. When the sample is
scanned at a small distance below the aperture, the optical resolution of
transmitted or reflected light is limited only by the diameter of the aperture.
The optical resolution attainable is in the range of 60e100 nm. The optical
image is generated by scanning the sample’s surface point by point and line
by line. A standard SNOM setup is shown in Fig. 1.3 [10].
n Advantages
o High resolution (up to 25 nm)
o Analysis of various properties made possible through contrast
o No special sample preparation needed
o Can be used for different kinds of samples (conductive, noncon-
ductive, and transparent)
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