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E344: Materials Processing - 06 - Materials Characterization Methods

This document provides an overview of several materials characterization methods, including diffraction techniques, microscopy, and microstructure analysis. Specifically, it discusses Bragg's law and how it relates experimental diffraction data to interplanar spacing in materials. It also explains how microscopy can be used to calculate mean grain diameter and determine phase content, composition, and other microstructural features at various length scales down to the atomic level. The document compares techniques like optical microscopy, scanning electron microscopy, transmission electron microscopy, and diffraction methods and discusses their typical resolution limits and applications in materials science.

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43 views

E344: Materials Processing - 06 - Materials Characterization Methods

This document provides an overview of several materials characterization methods, including diffraction techniques, microscopy, and microstructure analysis. Specifically, it discusses Bragg's law and how it relates experimental diffraction data to interplanar spacing in materials. It also explains how microscopy can be used to calculate mean grain diameter and determine phase content, composition, and other microstructural features at various length scales down to the atomic level. The document compares techniques like optical microscopy, scanning electron microscopy, transmission electron microscopy, and diffraction methods and discusses their typical resolution limits and applications in materials science.

Uploaded by

oates151
Copyright
© © All Rights Reserved
Available Formats
Download as PDF, TXT or read online on Scribd
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1

RichardE.Eitel
AssociateProfessor
Email:[email protected]
Office:Burchard 307B
DepartmentofChemical
EngineeringandMaterials
Science
StevensInstituteofTechnology
E344:MaterialsProcessing
06 MaterialsCharacterization
Methods
Theoverallobjectivethislectureistogiveyoutheskillstoapply
severalofthemostwidelyusedmaterialscharacterization
methods:
Bytheendofthislectureyoushouldbeableto:
Calculateinterplanar spacings in
materialspossessingacubic
crystalstructure.
UseBraggsLawtorelate
experimentaldiffractiondata
tointerplanar spacing.
Calculatemeangraindiameter
andATSMgrainsizefrom
microstructureimages.
2
Diffractionistheapparentbendingofwavesaroundsmallobjects
andthespreadingoutofwavebeyondsmallopenings.
BeyondanOpening
AroundACorner
Theapparentspreadingduetodiffractiondependsonthe
wavelengthofthewaveorparticle.
SpreadingofWhiteLightSource
DispersionofSoundWaves?
3
Youngsdoubleslitexperimentrevealedunexpected
propertiesoflightandquicklymovingparticles.
https://www.youtube.com/watch?feature=player_detailpage&v=Iuv
6hY6zsd0
Theperiodicityofinterferencepatternsproducedby
diffractionexperimentsarerelatedtothegeometryofthe
slitorstructurecreatingthepattern.
4
GuidedInquiryI:BraggsLaw
(10minutes)
Ifconstructiveinterferenceoccursfromtwoplanesof
atomsforascatteringangle(theta)of20.0degrees
whatisthedistance(d)betweentheplanes,ifthethe
wavelengthofthewavesis0.154nm?
A. 0.450nm
B. 0.225nm
C. 0.119nm
D. 0.0843nm
E. Idontknow
ConceptCheck:
5
Theconditionforconstructiveinterferencefromequally
spacedlayersisgivenbyBraggsNoblePrizeWinningLaw.
ConstructiveInterferencefor
ABC=n*lambda
1912@21YearsOld!

d
WhataretheconditionsforwhichdiffractionOccurs?
nz = 2 J sin 0
Considern=1
z
2J
= sin 0
6
Whataretypicalspacings (dspacings)betweenatomic
planes?
SimpleRelationshipsexistdepending
onthecrystalsystemofthecrystal
structure:
General(othorhomic)
1
d
hk|
2
=
h
2
a
2
+
k
2
h
2
+
|
2
c
2
Cubic(a=b=c):
1
d
hk|
2
=
h
2
+ k
2
+ |
2
a
2
d
hk|
=
a
h
2
+ k
2
+ |
2
Tetragonal a = h = c :
1
d
hk|
2
=
h
2
+ k
2
a
2
+
|
2
c
2
GuidedInquiryII:Interplanar Spacings
(10minutes)
7
Diffractionexperimentscanbeusedtodescribethestructureand
atomicpositionsinbothsingleandpolycrystalmaterials.
PowderDiffractionwithArea
Detector
SingleCrystalDiffraction
Powderdiffractionisusedtocollectdataonthefullsetof
interplanar spacingbyequallysamplingallorientations.
PhotographicMethod DigitalMethod
8
GuidedInquiryIII:DiffractionExperiments
(10minutes)
Dependingonthecrystalstructurenotallsetofplanes
producediffractionevents.
9
Microscopyisusetorecordgeometricalstructureand
orientationofmaterialsatthemicroscopicscale(<1mm).
GrainSize&shape
PhaseContent&Arrangement
CompositionandOrientation
FractureSurfaceand
FailureAnalysis
Theabilitytoobservesmallfeaturesisdiffractionlimitedby
thewavelengthoftheradiationused.
DiffractionPatternProduce
byPointlightsource
Resolution(R)islimitedbythe
overlapbetweenAirydisks:
R =
o
2
=
u.61z
p sino
p = InJcx o Rcroction o mcJio
sino = lcns gcomctry
AiryDisk
10
Opticalmicroscopesusevisuallighttocreateimagesand
characterizetheopticalpropertiesofmaterials.
PracticalResolutionLimit:
~1micron
IdentificationofMineralsby
OpticalProperties:
BoneCancer
Cell
Image:Nikon
2012SmallWorld
Intransmissionelectronmicroscopyhighenergyelectrons
areusetoachieveatomicscaleimagesofthin(~10nm)
sectionsofmaterial.
ResolutioninaTEM:
HighEnergyElectrons:
z
c
-
1
E
@300KeV
z
c
~ 2.u pm
Schematic
Practical
Resolutionlimit:
0.08nm~1
11
TEMscanbelargebutarealwaysEXPENSIVE!
HVEMJEOL1.25MeV
FEITitan300KeV
>$3MILLIONUSD??
Scanningelectronmicroscopeelectronicallyacquireanimageby
scanning(rastering)afocusedbeamofelectronsacrossasample
surface.
Resolutionlimit:
ProbeSize
Interactionvolume
~1nm
12
Scanningelectronmicroscopesarehavebecometheworkhorse
microscopeofchoiceforroutinematerialscharacterization
MinimalSamplePrep
CompatiblewithSizeofFeatures
ReasonableCost:
$100K500K
Thechoiceofmicroscopicmethodsdependsonthescale
andtypeofinformationtheisneeded!
ThefollowingareimagesofCarbonnanotubes:
OpticalMicroscope(Fluorescence):
30Mnanotubefilamentusedfor
solarenergyharvesting
ScanningElectronMicroscope:
Bundlesofnanotubes.
TransmissionElectron
Microscope:
atomicspacinginasingle
multiwallnanotube
13
MicrostructureAnalysis

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