Table Of ContentSpectroscopic Methods for
Nanomaterials Characterization
Volume 2
Edited by
Sabu Thomas
Raju Thomas
Ajesh K. Zachariah
Raghvendra Kumar Mishra
Elsevier
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List of Contributors
Rameshwar Adhikari
Tribhuvan University, Kathmandu, Nepal; Nepal Polymer Institute (NPI), Kathmandu,
Nepal
BasheerAhamed
B.S. Abdur Rahman University, Chennai, India
Gudimamilla Apparao
Acharya Nagarjuna University, Guntur, India
Anjali Bishnoi
Indian Institute of Technology HauzKhas, New Delhi, India
Jayesh Cherusseri
Indian Institute of Technology Kanpur, Kanpur, India
KuppannaChidambaram
VIT University, Vellore, India
YogeshS. Choudhary
Indian Institute of Space Science and Technology, Thiruvananthapuram, India
Andrea Delfini
Sapienza University of Rome, Rome, Italy
Kalim Deshmukh
B.S. Abdur Rahman University, Chennai, India
Aastha Dutta
Maharashtra Institute of Technology, Aurangabad, India
Jianwu Fang
Chang’an University, Xi’an, People’s Republic of China
Gejo George
HLL Lifecare Limited, Trivandrum, India
Sony George
University of Kerala, Trivandrum, India
Gurram Giridhar
Acharya Nagarjuna University, Guntur, India
Sven Henning
Fraunhofer Institute for Microstructure of Materials and Systems (IMWS), Halle/Saale,
Germany
Saravanakumar Jagannathan
Universiti Teknologi Malaysia, Johor Bahru, Malaysia
Nebu John
University of Kerala, Trivandrum, India;Mar Thoma College, Tiruvalla, India
xiii
xiv List of Contributors
LavanyaJothi
Indian Institute of Space Science and Technology, Thiruvananthapuram, India
Jithin Joy
Newman College, Thodupuzha, India
R.R.K.N. Manepalli
The Hindu College, Machilipatnam, India
Mario Marchetti
Sapienza University of Rome, Rome, Italy
Marta Marszalek
Institute of Nuclear Physics Polish Academy of Sciences, Krakow, Poland
Davide Micheli
Sapienza University of Rome, Rome, Italy
Goerg H. Michler
Martin Luther University Halle-Wittenberg, Halle/Saale, Germany
Raghvendra Kumar Mishra
Mahatma Gandhi University, Kottayam, India
Gomathi Nageswaran
Indian Institute of Space Science and Technology, Thiruvananthapuram, India
Khadheer S.K. Pasha
VIT University, Vellore, India
RobertoPastore
Sapienza University of Rome, Rome, Italy
DeepalekshmiPonnamma
Qatar University, Doha, Qatar
ShaohuaQu
Northwestern Polytechnical University, Xi’an, People’s Republic of China
P.S. RamaSreekanth
National Institute of Science and Technology, Odisha, India
Kishor K. Sadasivuni
Qatar University, Doha, Qatar
SowmyaSankaran
B.S. Abdur Rahman University, Chennai, India
Fabio Santoni
Sapienza University of Rome, Rome, Italy
Mengtao Sun
University of Science and Technology Beijing, Beijing, People’s Republic of China;
Chinese Academy of Sciences, Beijing, People’s Republic of China
Sabu Thomas
Mahatma Gandhi University, Kottayam, India
List of Contributors xv
AntonioVricella
Sapienza University of Rome, Rome, Italy
Liuding Wang
Northwestern Polytechnical University, Xi’an, People’s Republic of China
Runcy Wilson
HLL Lifecare Limited, Trivandrum, India
GuangleiWu
Qingdao University, Qingdao, People’s Republic of China
HongjingWu
Northwestern Polytechnical University, Xi’an, People’s Republic of China
Hui Xing
Northwestern Polytechnical University, Xi’an, People’s Republic of China
Duyang Zang
Northwestern Polytechnical University, Xi’an, People’s Republic of China
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
needsofresearchers withinthecountryandabroad.Hehasmorethan700
publications, 50 books, H Index-78 and 3 patents to his credit. He is a
reviewer to many international journals. Professor Thomas has attained
5thPositioninthelistofMostProductiveResearchersinIndiain2008e16.
Professor(Dr.)RajuThomasiscurrentlyViceChancellorofMiddleEast
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 12years 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,
xvii
xviii Editor Biographies
Germany. He has widely studied the kinetics of curing, morphology
development, and structural characteristics of in situ-cured
nanocompositesbasedonepoxyresinandreactiverubbers.Hisresearchis
reflectedinhissixpublishedresearcharticlesininternationaljournals,and
additional articles which are currently under review. In addition, many
articleshavebeenpublishedinpopularjournals.Hehasco-authoredmany
chapters and is co-editor of a book entitled Micro and Nanostructured
Epoxy/Rubber Blends which was recently published by Wiley and Sons.
He hasattended manynationaland 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
ofnanoscienceandnanotechnology.
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,forexample,EnvironmentalChemistryLetters(Springer).Hehas
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 xix
processing.Inaddition,hespecializesinpolymers,whichincludepolymer
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,andatomicforcemicroscopy(AFM).
1
Chapter
Atomic Force Microscopy as a
Nanoanalytical Tool
RameshwarAdhikari1,2, Sven Henning3and GoergH. Michler4
1TribhuvanUniversity,Kathmandu,Nepal;2NepalPolymerInstitute(NPI),Kathmandu,Nepal;3FraunhoferInstitutefor
MicrostructureofMaterialsandSystems(IMWS),Halle/Saale,Germany;4MartinLutherUniversityHalle-Wittenberg,
Halle/Saale,Germany
CHAPTEROUTLINE
1.1 Introduction 1
1.2 Specimen Preparation 7
1.2.1 ThinFilms 7
1.2.2 PhysicalandChemicalEtching, IonEtching 7
1.2.3 Ultramicrotomy 8
1.3 Typical Examples of Nanomaterials Characterization by Atomic Force
Microscopy 8
1.3.1 Nanoparticles ImagingandManipulation 8
1.3.2 BiobasedNanomaterials andNanoencapsulation 10
1.3.3 Comparison With ElectronMicroscopy 12
1.4 Concluding Remarks 14
Acknowledgments 15
References 15
1.1 INTRODUCTION
Asthedevelopmentofnewmaterialshasplayedaconsiderableroleinthe
advancement of human civilization, microscopic techniques have offered
probably the most important contribution toward the development of the
newmaterialsthemselves.Themicroscopedeliversthemostdirectinforma-
tion on the structure and properties of materials on different length scales,
not only allowing the experimentalist to interpret the correlation between
SpectroscopicMethodsforNanomaterialsCharacterization.http://dx.doi.org/10.1016/B978-0-323-46140-5.00001-7
Copyright©2017ElsevierInc.Allrightsreserved. 1
CHAPTER 1 Atomic Force Microscopy as a Nanoanalytical Tool
2
veryinternalstructuresofthematerialsandtheirpropertiesbutalsopermit-
tingtheinnovatortodesignnewstructuresrelevantfortargetedspecificap-
plications. In this regard, the electron microscope, and more recently the
scanning probe microscope (SPM), have been developed as reliable tools
for the characterization of nanomaterials. It should be noted that different
scattering techniques, in particular the X-ray methods, have made signifi-
cant contributions to the understanding of the structureeproperty correla-
tions of the materials, although the information is averaged over a large
volume. An SPM not only can access the structure of materials in the
macroscopic to nanoscale range but also studies various phenomena such
as adhesion, friction, electrical, magnetic, mechanical, and thermal proper-
ties of the materials on a very local level.
Owing to their ability to offer nanoscale resolution and versatile applica-
bility, SPM techniques have emerged as an indispensable nanomaterials
characterization tool. The invention of the first atomic force microscope
by Binnig and its introduction by Binnig et al. [1,2] in 1986 opened up
the possibility of obtaining surface images with atomic resolution on con-
ductorsandinsulatorsbyutilizingverysmalltipesampleinteractionforces.
Thus,amongtheSPMtechniques,theAFMisahighlyversatileandpopular
nanoanalytical tool. Thus, it has been common practice in past decades to
supplementelectronmicroscopywiththeAFM.
A brief survey of the fundamentals and relevant applications of this tech-
nique in nanomaterials research is presented in this chapter. For a detailed
accountofthefundamentalsandapplicationofAFMtechniquesappliedto
different materials, the readers may consult more concise reviews [3e7].
Inatomicforcemicroscopy,thesolidsurfacesarescannedinarasterpattern
by an extremely sharp mechanical probe attached to a cantilever. Highly
localized tipesample interaction forces are measured as a function of the
specimen’s local position. In its basic function, AFM provides high-
resolution imaging of the surface relief of the specimen between lateral
scalesofafewnanometerstoaboutahundredmicrometersasdemonstrated
by some examples presented in Fig.1.1.
Fig.1.1presentstapping-modeAFMimagesofdifferentmagnificationsof
thin isotactic polypropylene (iPP) film sandwiched between polystyrene
(PS) layers prepared by the microlayer coextrusion technique [8e10]. The
most popular AFM mode of operation is the so-called “tapping” mode or
“intermittent-contact”mode,inwhichthesampleisscannedwithanoscil-
lating probe. The contrast mechanism in the AFM operation is based on
thelocalmechanicalpropertiesofthespecimen[11e14].
