ELECTRON MICROSCOPY - unl.edu MICROSCOPY.pdf · Electron Energy Loss Spectroscopy andEd Energy-Filt...
Transcript of ELECTRON MICROSCOPY - unl.edu MICROSCOPY.pdf · Electron Energy Loss Spectroscopy andEd Energy-Filt...
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ELECTRON MICROSCOPYWednesdays at One
UNL REU in Nanomaterials and Nanoscience
Jeff ShieldDepartment of Mechanical Engineering
University of Nebraska
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What we can discoverWhat we can discover . . .IMAGING
M ifi ti f l illi•Magnifications of several million times•Resolution approaching 0.1 nm
DIFFRACTIONDetermine crystal pp g
•See defects such as grain boundaries, dislocations, stacking faults etc
structureSmall areas (<1 nm)3-D symmetrystacking faults, etc.
•3-D imaging3 D symmetry
CHEMISTRYDetermine what elements are thereDetermine concentrationDetermine concentrationSmall areas (<1 nm)
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The PartsThe Parts . . .
1 Electron source1. Electron source2. Electromagnetic lenses3 D t ti3. Detection
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The Electron SourceThe Electron Source
“W k F ti ”e-“Work Function”
e-
e
e-
Free e-
e-
e-
e-
Two techniques to overcome the work function
Vacuum
Solid
1. Thermionic emission2. Field emission
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Thermionic EmissionThermionic Emissione- Use thermal energy
e-
e
e-
Use thermal energy
iFree e-
e-
e-
e-
i
Vacuum
Solide-ee-Electron beam
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Field EmissionField Emissione- Use electric field
e-
e
e-
Use electric field--modifies barrier
e
Free e-
e-
e-
e-
Vacuum
Solide-ee-Electron beam
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Field v ThermionicField v. Thermionic
Fi ldField•Smaller virtual source (=smaller beam size)•More uniform electron energy (easier to control)
Thermionic•Less stringent vacuum requirementsLess stringent vacuum requirements•Cheaper
Field emission sources provide higher resolution, better spectroscopy
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EM LensesEM Lenses
• CondensorCondensor– Demagnify electron beam
Objective• Objective– Focus probe onto sample (SEM)
( )– Focus image (TEM)• Magnifying (only in TEM)
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Scanning Electron Microscopy (SEM)
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SEMSEM
Electron GunX-ray DetectorElectron Detector(s)
Column (lenses)
Sample Chamber
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Detection: SEMDetection: SEMX-rays
Backscattered electronsSecondary electrons Auger electrons
Electron beam
Can be microns!
Interaction volume depends on:Interaction volume—depends on:•Accelerating voltage•Atomic number of sample•Density of material
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SEM OperationSEM OperationElectron Beam
Scan Area
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Secondary electronselectrons
Low energyUsed to form most iimages
Auger electronsLow energyElement-specificElement specificCarry chemical information
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More secondary electron images
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Backscattered electronsHigh energy beam electronsg gyCarry atomic number information
Al Ca Cl
Fe K Mg Na
X-raysCarry chemical information
(images from EDAX, Inc.)
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SEM: SummarySEM: Summary
• Magnification depends on scanned areaMagnification depends on scanned area• Resolution depends on probe size and
electron specimen interactionelectron-specimen interaction• Good for fracture surfaces, microstructure,
ti l tparticles, etc.• Easy to interpret images!
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Transmission Electron Microscopy (TEM)
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Transmission Electron Microscopy (TEM)
El t GElectron Gun
Condenser Lenses
S l Ch b /Obj ti LSample Chamber/Objective Lens
Magnification Lenses
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Detection: TEMDetection: TEMX-rays
Backscattered electronsSecondary electrons Auger electrons
Electron beam
<100 nm!
Interaction volume
<100 nm!
Interaction volume•Much smaller than in SEM!!!
•Able to probe smaller regions!!!Diffracted electrons
Transmitted electrons
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ImagingImagingCondensor lens
<100 nm!
Beam now hits large area
<100 nm!
Diffraction Plane
Image Plane
Diffraction Plane
Magnifying lenses
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“Regular” ImagingRegular Imaging“Bright Field”
Contrast due to:•Differences in grain orientation•Imperfections in crystals
100 nm
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“Regular” ImagingRegular Imaging
(a) (b)
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High-Resolution ImagingHigh Resolution ImagingContrast due to wave interaction•“See” columns of atoms• See columns of atoms
From Urban, MRS Bulletin 32, 946 (2007)
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High-Resolution ImagingHigh Resolution Imaging
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DiffractionSelected area electron diffraction
Nanoprobe and/or convergent beam electron diffraction
Crystal structure determination
Small region ORSmall region OR3D symmetry (point group)
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Chemical AnalysisChemical Analysis
e- e-ΔEe
e-
eΔE
e-
e-
Incoming electrons ionize atomsRelaxation leads to emission of x ray
e-
e-
Relaxation leads to emission of x-rayCharacteristic of atom•Collect x-rays and categorize them by energy
X-ray
“ENERGY DISPERSIVE X-RAY SPECTROSCOPY (EDS)”
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An ExampleAn Example . . .1000
ount
s
Ti
500
mbe
r of C
o
00 10 20 30 40
Nu
10.00
nts
100 nmElectron probe 6.00
8.00
nds
of C
ou Fe
1.5 nm2.00
4.00Th
ousa
n
0.000 10 20 30 40
Position (nm)
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Electron Energy Loss Spectroscopy d E Filt d I iand Energy-Filtered Imaging
e- e-e
e-
eE = Eo - Eion
e-
e-
Incoming electrons ionize atomsIncoming electron loses energy corresponding to the
e-
e-
Incoming electron loses energy corresponding to the ionization energy of the atom
“Energy loss spectra”•Form image using specific electrons
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Electron Energy Loss Spectrumgy pns
ityIn
ten
Peaks due to energy loss during Fe K shell ionization
Energy loss
EELS provides information about:Elements in samples (especiall good for lo Z elements)•Elements in samples (especially good for low Z elements)
•“Neighborhood” of each atom (bonding type, valence, etc)
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Energy Filtered TEM (EFTEM)Energy Filtered TEM (EFTEM)Select specific electrons to form imageThen, see where those electrons have been
Bright fieldBright field
Energy nsity Fe windowFe window
50 nm50 nm
gy“window”
Inte
n
Fe50 nm50 nm
Energy loss
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TEM: SummaryTEM: Summary
• Resolution depends on lenses electronResolution depends on lenses, electron source
• Good for seeing small things• Good for seeing small things• Good for analyzing imperfections• Combine microstructure (imaging), crystal
structure analysis (diffraction) and chemical analysis (EDS/EELS) in one instrument
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Electron MicroscopyElectron Microscopy
Lots more stuff possible!!!Lots more stuff possible!!!• Electron Holography• Electron energy loss spectroscopy• Scanning Transmission Electrong
Microscopy (STEM)