1-x-ray introduction
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ADVANCED
NANOMATERIALS CHARACTERIZATION
I
UNIT I XRAY DIFFRACTION
Xraypowderdiffraction
Singlecrystaldiffractiontechniques
Determinationofaccuratelatticeparameters
Nanostructural analysis
ParticlesizeanalysisusingSchererformula
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Moretools
Otherstakepicturesinthemomentumspaceorwavevectorspaceratherthaninrealspace:
XRD (XRayDiffraction)
LEED(Low EnergyElectron Diffraction)
RHEED (Reflection High EnergyElectron Diffraction)
NEUTRONDIFFRACTION
Aswith
any
camera,
information
isreadily
obtained
about
thestaticstructureofthematerial,althoughblurrinessalsoconveyssomedynamicalinformation
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Somemore!
Additionally, therearesomeothertoolsalsothatworkintherealtimeandinthefrequencyvariablespace
Intherealtime timede endentluminescentstudiescanbeusedtostudythedynamicalevolutionofthesystem
Inthefrequencyspacearetheopticalspectrospcopies:
IR,VIS andUV Spectroscopies
Light Scattering,Ellipsometry,IRabsorption,Raman Scattering,
P oto uminescencean NonLinear Optica Spectroscopy
EELS(Electron EnergyLoss Spectroscopy)
AES (Auger Electron Spectroscopy)
INS(Inelastic Neutron Scattering)9/23/2009 6
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Evenmore!!
Techniquesinwhichbothelectronsandphotonsplayasignificantrole:
EXAFS(ExtendedXrayAbsorption FinestructureSpectroscopy)
XPS (XrayPhotoemission Spectroscopy)
UVPS (UV Photoemission Spectroscopy)
NMR(Nuclear Ma netic Resonance)
ESR(Electron Spin Resonance)
NQR(Nuclear Quadrupole Moment )
MOSSBAUEREFFECT9/23/2009 7
Herewe
go
again!!!
Usin ionic robessomemoretechni ues:
o SIMS (SecondaryIon Mass Spectrometry)
o RBS (Rutherford Back Scattering)
o PAS (PositronAnnihilation Spectroscopy)
o uon recess on pec roscopy
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WilhelmConradWilhelmConrad
RntgenRntgen((1845184519231923))
Wilhelm Conrad Rntgen
discovered the X-rays in
1895.
n e was onoure wthe Nobel prize for physics.
In 1995 the German FederalMail edited a stamp dedicated
to W. C. Rntgen.A modern radiograph
of a handBertha Rntgens Hand
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Radiographsliketheonesinthelastslidearesimplyshadowgrams.
TheXrayseitherpassstraightthroughorarestoppedbytheob ect.
Thediagramontheupperleftillustratestheprincipleandshowsaperfectshadow.
Inreality,alargefractionoftheXraysarenotsimplyabsorbedortransmittedbytheobjectbutarescattere .
Thediagramonthebottomleft
illustratesthiseffectandillustratesthefuzzyedgeoftheobjectthatisproducedintheimagebythescatteredXrays.
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Thefirstkindofscatterprocesstobe
recognisedwasdiscoveredbyMaxTheodorFelixMaxTheodorFelixvonvon LaueLaue
LauewasawardedtheNobelprizefor
physicsin1914"forhisdiscoveryoftheforhisdiscoveryofthe
diffractionofXdiffractionofXraysbycrystalsraysbycrystals".
HiscollaboratorsWalterFriedrichandPaul
Knipping in1912,tookthepictureof a
characteristicpatternofacrystal(copper
sulphateinthiscase)whenitscattereda
beamofXrays.
Max Theodor Felix von Laue
(1897-1960)
TheXraypowderdiffractionpatternofa
puresubstanceislikeafingerprintofthe
substanceandisthusideallysuitedfor
characterizationandidentificationof
polycrystallinephases.9/23/2009 12
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X rays are invisible, highly penetrating electromagnetic radiationof much shorter wavelength (higher frequency) than visible light
The wavelength range for X rays is from about 10 m to about1011 m and the corresponding frequency range is from about3 1016 Hz to about 3 1019 Hz
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X-RAY ENERGY Electromagnetic radiation is described as having packets of
energy, or photonsphotons
E=hE=h
andand
= c/= c/
The energy of the photon is related to its frequency by the
following formula
E=E=hchc//xxrrayay 1010
1010 11AA E E 101044eVeV
=Wavelength,=Wavelength, =Frequency, c=Velocityoflight=Frequency, c=Velocityoflight
E=
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X rays can be produced in a highly evacuated glass bulb,called an Xray tube, that contains essentially twoelectrodesan anode made of platinum, tungsten, oranother heav metal of hi h meltin oint and a cathode.
X-RAY TUBE
Evacuatedglassbulb
When a high voltage is applied between the electrodes,streams of electrons (cathode rays) are accelerated from thecathode to the anode and produce Xrays as they strike theanode.
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Anode Cathode
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K-shell knockout The free electron collides with the tungsten atom, knocking an electron out
of a lower orbital.
An electron in a higher orbital immediately falls to the lower energy level,
releasing its extra energy in the form of a photon. It's a big drop, so thehoton has a hi h ener level it is an X-ra hoton.
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Monochromatic and Broad Spectrum of X-rays
For X-rays to be generated, electrons of high energy (> 104)are required.
Some of these electrons may excite electrons from the corestates in the target metal, which then recombine, producinghighly monochromatic X-rays. These are referred to ascharacteristic X-ray lines.
Other electrons, which are decelerated by the periodicpotential of the metal, produce a broad spectrum of X-rayfrequencies (BremsstrahlungBremsstrahlung- stopping potential).
Depending on the diffraction experiment, either or both ofthese X-ray spectra can be used.
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Continuous
Radiation
(BremsstrahlungBremsstrahlung)
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CharacteristicRadiation
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XraySpectrum
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CharacteristicRadiation
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Absorption of X-rays The atoms that make up your body tissue absorb
visible light photons very well. The energy level ofthe photon fits with various energy differencesbetween electron positions.
Radio waves don't have enough energy to moveelectrons between orbitals in larger atoms, so theypass through most stuff.
X-ray photons also pass through most things, butfor the opposite reason: They have too muchenergy.
...somethingyouwon'tseeveryoften(Visible light)
Xray
e a sorp on o -rays s g ven yI (I () = ) = IIoo (( ) exp ( ) exp (xx))
Where,Where, absorption coefficient of the materialabsorption coefficient of the material
density of the materialdensity of the material
xx distance travelled by the Xdistance travelled by the X--rays through the materialrays through the material
Note that mass absorption coefficients are additive functions ofthe weights fractions of elements.
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Absorption of X-rays A largerlarger atomatom is more likelylikely toto absorbabsorb anan XXrayray photonphoton in
this way, because larger atoms have greater energy
matches the energy of the photon.
SmallerSmaller atomsatoms, where the electron orbitals are separated byrelatively low jumps in energy, are lessless likelylikely toto absorbabsorb XXrayrayphotonsphotons.
The soft tissue in your body is composed of smaller atoms,and so does not absorb Xray photons particularly well.
The calcium atoms that make up your bonesbones are much larger,so they are better at absorbing Xray photons.
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