Table Of ContentSurender Kumar Sharma Editor
Dalip Singh Verma
Latif Ullah Khan
Shalendra Kumar
Sher Bahadar Khan Associate Editors
Handbook
of Materials
Characterization
Handbook of Materials Characterization
Surender Kumar Sharma
Editor
Dalip Singh Verma • Latif Ullah Khan
Shalendra Kumar (cid:129) Sher Bahadar Khan
Associate Editors
Handbook of Materials
Characterization
123
Editor
SurenderKumarSharma
DepartmentofPhysics
FederalUniversityofMaranhão
SãoLuis,Maranhão,Brazil
AssociateEditors
DalipSinghVerma LatifUllahKhan
DepartmentofPhysics&Astronomical BrazilianNanotechnologyNational
Science Laboratory(LNNano)
CentralUniversityofHimachalPradesh BrazilianCenterforResearchin
Dharamshala,Kangra EnergyandMaterials(CNPEM)
HimachalPradesh,India Campinas,SãoPaulo,Brazil
ShalendraKumar SherBahadarKhan
DepartmentofAppliedPhysics CenterofExcellencefor
AmitySchoolofAppliedSciences AdvancedMaterialsResearch
AmityUniversityHaryana KingAbdulazizUniversity
Gurgaon,India Jeddah,SaudiArabia
ChemistryDepartment
FacultyofScience
KingAbdulazizUniversity
Jeddah,SaudiArabia
ISBN978-3-319-92954-5 ISBN978-3-319-92955-2 (eBook)
https://doi.org/10.1007/978-3-319-92955-2
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Preface
One of the significant aspects of materials-based research is the characterization
tools. Today, there is an immense range of scientific techniques available that
enables us to study physiochemical properties of the materials. This book focuses
ontheutmosteffectiveandwidelyusedtechniquesavailableforstructural,morpho-
logical, and spectroscopic characterizations of materials. Three important aspects
ofcharacterizationnamelymaterialsstructures,morphology,andchemicalanalysis
areincludedinthepresentvolume.Thedevelopmentsinwiderangeoftechniques
and their application to the quantification of the materials properties are essential
sidesofthebook.
The principal objective is to provide a concise reading material on both prac-
tical and theoretical description of the techniques used to characterize a wide
varietyofmaterials.Ourapproachisfocusedonfundamentalunderstanding,basic
instrumentation, experimental strategy, analyses, and application part. Most of the
characterization techniques are used throughout undergraduate courses; however,
the background of these methods will not be provided in the standard textbooks.
This book will serve as an overview of characterization of materials for a wide
audience: from beginners and graduate-level students up to advanced specialists
in both academic and industrial sectors. The authors of each chapter have been
encouraged to present the highlights from the extensive literature on the topic
includinglatestcutting-edgeresearchusingbothconventionalandnonconventional
characterizationtools.
SãoLuis,Brazil SurenderKumarSharma
v
Contents
1 NeutronDiffraction:AtoolfortheMagneticProperties .............. 1
PabloLeiteBernardoandHelioSalimdeAmorim
2 Small-AngleX-RayScatteringtoAnalyzetheMorphological
PropertiesofNanoparticulatedSystems................................. 37
Oscar Moscoso Londoño, Pablo Tancredi, Patricia Rivas,
DiegoMuraca,LeandroM.Socolovsky,andMarceloKnobel
3 DynamicLightScattering:EffectiveSizingTechnique
forCharacterizationofMagneticNanoparticles........................ 77
SimSiongLeong,WeiMingNg,JitKangLim,andSweePinYeap
4 ScanningElectronMicroscopy:PrincipleandApplications
inNanomaterialsCharacterization....................................... 113
Kalsoom Akhtar, Shahid Ali Khan, Sher Bahadar Khan,
andAbdullahM.Asiri
5 TEMforAtomic-ScaleStudy:Fundamental,Instrumentation,
andApplicationsinNanotechnology ..................................... 147
YasirJaved,KhuramAli,KanwalAkhtar,Jawaria,M.IrfanHussain,
GulzarAhmad,andTaskeenArif
6 Materials Characterization Using Scanning Tunneling
Microscopy:FromFundamentalstoAdvancedApplications ......... 217
Suryakanti Debata, Trupti R. Das, Rashmi Madhuri,
andPrashantK.Sharma
7 Atomic and Magnetic Force Studies of Co Thin Films
andNanoparticles:UnderstandingtheSurfaceCorrelation
UsingFractalStudies....................................................... 263
IndraSulania,R. P.Yadav,andRanjeetKumarKarn
vii
viii Contents
8 OpticalSpectroscopyandItsApplicationsinInorganicMaterials... 293
MarcioAurélio PinheiroAlmeidaandAdeiltonPereiraMaciel
9 Fourier Transform Infrared Spectroscopy: Fundamentals
andApplicationinFunctionalGroupsandNanomaterials
Characterization............................................................ 317
Shahid Ali Khan, Sher Bahadar Khan, Latif Ullah Khan,
AliyaFarooq,KalsoomAkhtar,andAbdullahM.Asiri
10 Rare Earth Luminescence: Electronic Spectroscopy
andApplications............................................................ 345
LatifUllahKhanandZahidU.Khan
11 RamanSpectroscopy:APotentialCharacterizationTool
forCarbonMaterials....................................................... 405
PadmnabhRaiandSatishKumarDubey
12 Photoelectron Spectroscopy: Fundamental Principles
andApplications............................................................ 435
JagdishKumar
13 Introduction to X-Ray Absorption Spectroscopy and Its
ApplicationsinMaterialScience.......................................... 497
AdityaSharma,JitendraPalSingh,SungOkWon,KeunHwaChae,
SurenderKumarSharma,andShalendraKumar
14 31PSolid-StateNMRSpectroscopyofAdsorbedPhosphorous
Probe Molecules: Acidity Characterization of Solid Acid
CarbonaceousMaterialsforCatalyticApplications.................... 549
BhaskarGarg
Index............................................................................... 597
Chapter 1
Neutron Diffraction: A tool for the
Magnetic Properties
PabloLeiteBernardoandHelioSalimdeAmorim
1.1 Introduction
Experimental techniques based on neutron scattering have a special relevance in
the study of new materials due to some basic aspects of the neutrons as particles
in free state, that is, outside the atomic nucleus. They are relatively stable, with
a mean lifetime of about 14min; as indicated in their own name, do not have a
net electric charge, that is, they are neutral; have no measurable electrical dipole
moment; but have a relevant magnetic dipole moment associated with an intrinsic
angularmomentumorspin.
Because they do not have an electric charge, or an electric dipole, they do not
electricallyinteractdirectlywithatoms,ions,ormoleculesthatmakeupmatter.In
general,theyarepoorlyabsorbedindirectinteractionwithmatterwhencomparedto
otherchargedparticlesorevenwithX-andgamma-typephotons.Thepredominant
interaction is with the atomic nuclei. The exact form of the interaction between
neutronsandnucleiisnotknown,butitispossibletotheoreticallytreattheproblem
with Fermi’s pseudo-potential. We will detail this later. This interaction can occur
in an elastic regime where the kinetic energy of the neutron is conserved in the
collisionwiththenucleus.Weusuallycalltheelasticscatteringregimeasneutron
diffraction,andthephenomenonofthecollectiveneutronscatteringofasetofatoms
canbetreatedinwavebases,involvingnotions,suchasconstructiveanddestructive
interference.
P.L.Bernardo((cid:2))
CentroBrasileirodePesquisasFìsicas(CBPF),RiodeJaneiro,Brazil
e-mail:[email protected]
H.S.deAmorim
UniversidadeFederaldoRiodeJaneiro(UFRJ),RiodeJaneiro,Brazil
e-mail:[email protected]
©SpringerInternationalPublishingAG,partofSpringerNature2018 1
S.K.Sharma(ed.),HandbookofMaterialsCharacterization,
https://doi.org/10.1007/978-3-319-92955-2_1
2 P.L.BernardoandH.S.deAmorim
Neutron diffraction experiments are widely used for the determination, and
refinement, of crystalline structures. They are applied in materials in the form of
monocrystalsorpolycrystals(powder)throughexperimentalmethods,andanalysis
procedures, that are completely similar to those used in X-ray diffraction. This
correspondence can be appreciated with the use of structural refinement programs
of polycrystalline materials by the Rietveld method, such as FullProf and GSAS
where,ingeneral,itispossibletoprocessneutrondiffractionandX-raydiffraction
dataonthesameplatformandwiththesamealgorithms.
Animportantfeatureinneutrondiffractionisthatthereisnotmuchcontrastinthe
efficiencyofscattering,ifsowecanexpressit,amongthevariouschemicalelements
in the periodic table. In X-ray diffraction, the scattering efficiency, as depicted by
theatomicscatteringfactor,increaseswiththenumberofelectronsintheatom.This
factallowsittobemucheasiertolocatelightatomsinassociationwithheavyatoms
through neutron diffraction experiments than X-ray diffraction. The advantages of
neutrondiffractioninrelationtoX-raydiffractioninthelocationofhydrogenatoms
present,forexample,inorganicmaterialsorinhydratedmaterials,arewell-known.
Intheinelasticscatteringregime,neutronscantransfermomentumtotheatoms
inthelattice.Inanuclearreactor,wecanproduceneutronswithenergyveryclose
to the vibrational energy of the atoms (thermal neutrons) and yet with wavelength
of the order of the interatomic distances. In this way, an expressive interaction
with normal crystal vibration modes (phonons) is possible, and the result of the
scattering can be very informative. Because they work with very close energies
between neutrons and phonons, neutron diffraction is a very skillful technique for
thestudyoflatticedynamics.
Anotherformoftheinteractionofneutronswithmatteristhemagneticinterac-
tion. Whenever atoms with permanent magnetic dipole moments are present, an
interaction between the atomic magnetic dipole and the magnetic dipole of the
neutron is established. Particularly important is the result of this interaction when
we have materials with some sort of magnetic ordering. The result of a neutron
diffractionexperiment,mediatedbymagneticinteraction,hasthepotentialtoreveal
the spatial arrangement of the magnetic dipoles of the magnetic sublattice present
inthematerial.Ontheotherhand,intheinelasticscatteringregimeintermediated
bythemagneticinteraction,wecanobserveenergytransfersbetweenneutronsand
spin waves present in the material in a manner analogous to that occurring in the
inelasticnuclearscatteringwiththelatticephonons.
Inthischapter,weintendtogivesomepracticalinformationonhowthischarac-
terizationcanbeachievedthroughacasestudy.Webeginwithasimpledescription
of the scattering of neutrons with nuclei where we try to give an overview of the
mostimportantconceptsinvolved,andthenwewilldiscussthemagneticscattering.
Naturally, it would be far from the scope of this chapter to attempt to synthesize
allthedetailsofthetheoreticalmodelingoftheneutronscatteringprocess,andfor
thosewhowouldappreciateagreaterdepth,werememberthattherearegoodtexts
thatdevelopallthetreatmentfromthefirstprinciples[1,2].
1 NeutronDiffraction:AtoolfortheMagneticProperties 3
1.2 NuclearScattering
Shortly after the discovery of the neutron by Chadwick in 1932, the first studies
on the possibility of the diffraction of a beam of neutrons by crystals, in the same
way that occurs with an electron or X-ray beams, appeared. The analogy is very
directandveryplausible.Neutronsareverymassiveparticleswithmasscomparable
to the hydrogen atom, and because they do not have a net electric charge, they
have a remarkable ability to penetrate the solid matter. According to the quantum
mechanics,eachparticleofmomentump=mv(m–mass,v–velocity)awaveof
wavelengthλgivenbytherelationofdeBroglie,
h
λ= (1.1)
p
where h is the Planck constant. If we consider a beam of neutrons generated by a
radioactive source incident on a paraffin-moderating target, we will have a disper-
sion of the kinetic energy of the neutrons by elastic collisions with the hydrogen
atoms, abundant in paraffin. This dispersion closely follows the distribution of
Maxwell–Boltzmann velocities for an ideal gas. If the absolute temperature of the
moderatingtargetisT,theaveragekineticenergyoftheneutrons(k)isgivenby
p2 3
K = = kT (1.2)
2m 2
wherekistheBoltzmannconstant.Foraparaffin-moderatingtargetatroomtemper-
ature(∼300K),theaveragekineticenergyoftheneutronsisabout0.04eVwitha
DeBrogliewavelengthofapproximately1.5˚A.Thisvaluecloselyapproximatesthe
averagewavelengthoftheKα doubletofanX-raytubewithcopperanode,widely
used in the X-ray diffractometers of polycrystals for structural characterization of
themostdiversematerials.
In1930sthefirstevidenceofneutrondiffraction[3–5]emergedthroughexper-
imentalassembliesbasedonlowintensityradioactivesources.Theapplicationsof
neutron diffraction in crystallography as an accessory technique in the structural
characterizationofmaterialshadtheirgreatimpetusinthepost-IIWarperiodwith
theadventofnuclearreactorsandacceleratorsofparticles.
With the new sources, it is possible to obtain beams with abundant thermal
neutrons.Theseneutronbeamshaveacontinuousspectrumofkineticenergy,which
is to say, in wavy terms, a “white” radiation. From a white beam of neutrons, we
canobtainamonochromaticbeamusingmonocrystalsexactlyasweproceedwith
X-rays. Monocrystals of Be, Si, Ge, Cu, Pb, or even laminar pyrolytic graphite
are used for this purpose. Figure 1.1 shows, schematically, an experimental setup
using a monochromatic beam for the study of a polycrystalline sample, in a
configurationequivalenttoDebye–ScherrergeometryusedbyX-raydiffractometers
for polycrystals. The differences are more related to the dimensions: the neutron
diffractometers are significantly larger than their equivalents for X-rays. In part,
