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Peter Ercius, Cornell University
3D Imaging of Nanostructures Using Electron Tomography, and the Impact
of Aberration Correctors
3D Imaging of Nanostructures Using Electron Tomography, and the Impact
of Aberration Correctors
Peter ErciusHuolin XinVarat IntaraprasonkDavid Muller
Applied and Engineering Physics, Cornell University
Lynne GignacIBM T.J. Watson Research Center, SRC
Peter Ercius, Cornell University
Tomographic ReconstructionTomographic ReconstructionGoal: 3D information from thick, crystalline, high atomic number materials
- Measure structure thicknesses, x-sections, CDsChallenges:
• Image intensities for electron tomography must be monotonic with thickness
Not Conventional TEM• Contrast reversal in HAADF Scanning TEM (Z-contrast)
High mass-thickness materials appear dark at high tilts
• Samples must be tilted to ±70° to recover 3D informationTilting causes translations and rotations between images that must be corrected (post-processing)
Impact of aberration correctors:• Lateral and depth resolution significantly improved
Depth resolution < sample thickness
Peter Ercius, Cornell University
For the best results:
• Acquire many images over as large a tilt range as possible
→ One every 1-2° from ±70°
→ Filling Fourier Space
Tomography ExperimentTomography Experiment
Acquisition
e-
Requires
Reconstruction:
• Accurate spatial alignment
• Determination of tilt axis
• Accurately spaced angular increments
Peter Ercius, Cornell University
V2 Via Liner Layer by HAADF STEMV2 Via Liner Layer by HAADF STEMEtch Roughness
LithographyRoughness
90nm Cu line width
Peter Ercius, Cornell University
Contrast Reversal in HAADF STEMContrast Reversal in HAADF STEM
Annular Dark Field detector
y
x
200 keV IncidentElectron Beam
(∆E≈0.6 eV)
1 atom wide (0.2 nm) beam is rasteredacross the sample to form a 2-D image
ADF image
Peter Ercius, Cornell University
Contrast Reversal with ThicknessContrast Reversal with Thickness
Cu via
• HAADF STEM• 0° tilt
Cu line
300nm
Cu via
Cu line
• HAADF STEM• 70° tilt
Peter Ercius, Cornell University
Why the Contrast Reversal in HAADF?Why the Contrast Reversal in HAADF?
0
0.2
0.4
0.6
0.8
1
0 0.5 1 1.5 2 2.5 3 3.5
Ta Cu Si
Nor
mal
ized
Inte
nsity
(a.u
.)
Target thickness (µm)
Signal drops when electrons scatter outsideouter angle of detector(e.g. backscattering)
But no electrons stop in the sample: Backscatter
DF
BF
200keVfor Cu in 500 mEKR µρ
γ ≅=
Peter Ercius, Cornell University
Maximum Material Thickness: HAADF vs IBFMaximum Material Thickness: HAADF vs IBFApparent thickness is increased ~threefold by tilting
t
tmax
70°
HAADF IBFTantalum 47 73±7
220±201160±30
Copper 143Silicon 855
Maximum material thickness, tmax (in nm), for ±70° tilt
Peter Ercius, Cornell University
IBF vs. HAADF for Cu: SNRIBF vs. HAADF for Cu: SNR
0
10
20
30
40
50
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
Contrast for 5nm thickness changesnormalized by Poisson noise
ADF (100-250R)IBF (0-100R)
SNR
Cu Thickness (µm)
ADF contrast reversal
• Question: when does IBF become advantageous over HAADF?– Compare for ∆t=5nm at relevant thicknesses
• IBF is better even before contrast reversal thicknesses are reached
Peter Ercius, Cornell University
Stress Void ReconstructionsStress Void ReconstructionsHAADF IBF
~500nm
Peter Ercius, Cornell University
Stress Void and Via ReconstructionStress Void and Via Reconstruction
Peter Ercius, Cornell University
Copper Line ResistivityCopper Line Resistivity
• By preparing one sample for tomography we can gain information about ~2nm slices of each line.
• Getting the same information by CTEM requires preparation and measurement of many samples.
2.4
2.6
2.8
3
3.2
9000 10000 11000
Conductor area vs. resistivity
Tomo slicesTomo meanTEM mean
Res
istiv
ity (µΩ
cm)
Cu area (nm2)
- TEM data from L. Gignac
Peter Ercius, Cornell University
Electron Lens AberrationsElectron Lens Aberrations
∆s = path difference due to wave aberration
C3=0C3>0
• Use circular aperture to cutoff electrons with a large phase shift ∆s across the lens
Peter Ercius, Cornell University
Balance Aberration and DiffractionBalance Aberration and Diffraction
α00d
• The image of a point transferred through a lens with a circular aperture of semiangle α0 is an Airy disk of diameter:• Balance spherical aberration against the aperture’s diffraction limit
• Less diffraction with a larger aperture• Design correctors to eliminate phase shift across the lens
• Lens aberrations are a non-convergent power series• Correct C3 C5 ; Correct C5 C7 ; ETC…
00 1 α∝d
Peter Ercius, Cornell University
Depth Point Spread Function (PSF)Depth Point Spread Function (PSF)C5 limited:C3 limited:
200nm z
x
nmz 33≈∆ nmz 6.3≈∆200keV, α=29.1mRadC3=-0.0842mm, C5=100mm, ∆f=-132Å
200keV, α=9.6mRad, C3=1.2mm, ∆f=550Å
Peter Ercius, Cornell University
Depth Sectioning by Focal SeriesDepth Sectioning by Focal Series
∆f0
∆f1
∆f2
∆f3
Peter Ercius, Cornell University
Prospects for Depth SectioningProspects for Depth Sectioning
1
10
100
0 20 40 60 80 100
100 kV200 kV300 kV
Dep
th o
f Foc
us (Å
)
Probe Forming Semi-Angle (mrad)
C3>0
C3~0
C5~0
Current STEM correctors: ∆z ~ 3-8 nm Super STEM: ∆z ~ 1 nm?
Peter Ercius, Cornell University
Tomography or Depth SectioningTomography or Depth Sectioning
0
0.2
0.4
0.6
0.8
1
0 2 4 6 8 10
Focal SeriesTilt Series
Nor
mal
ized
inte
nsity
(a.u
.)
Depth (nm)
Focal Series: Change defocus to sample at different depthsTilt Series: Tilt sample to fill Fourier-Space with projections
Peter Ercius, Cornell University
Information Limit for Depth SectioningInformation Limit for Depth Sectioning
0 0.5 1 1.5 2 2.5 3 3.5 4−0.05
−0.04
−0.03
−0.02
−0.01
0
0.01
0.02
0.03
0.04
0.05
kr (1/angstrom)
k z (1/
angs
trom
)
C3−limited, α
max = 10 mrad
C5−limited, α
max = 29 mrad
C7−limited, α
max = 49 mrad
Information limit: 0.05-1 = 20ÅHalf-angle:
kr cutoff:λαα
max
max
22
°°=
1.1 :covers55.mrad6.9
C3 limited:
°°=
32.3 :covers66.1mrad29
C5 limited:
Peter Ercius, Cornell University
Fourier Reconstruction with Depth Sectioning at Different Tilts
Fourier Reconstruction with Depth Sectioning at Different Tilts
0° -45°, 0°
kz
ky
-45°, 0°, 45°
±70° @ 7° inc.
Peter Ercius, Cornell University
Fourier Reconstruction MethodsFourier Reconstruction Methods
Focal & Tilt SeriesTilt Series
Peter Ercius, Cornell University
Convolution Simulation: PSFConvolution Simulation: PSFFocalSeries
Focal &Tilt SeriesTilt Series
z
y
200keV, C3=-0.0842mm, C5=100mm, f0=-132, α=29.1mRad±70° @ 7° increments
Peter Ercius, Cornell University
Spread of PSF IntensitySpread of PSF Intensity
0
0.2
0.4
0.6
0.8
1
0 1 2 3 4 5
Focal&TiltTilt
Nor
mal
ized
Inte
grat
ed In
tens
ity (a
.u.)
Distance from center (nm)
• Intensity is decentralized for both methods
Peter Ercius, Cornell University
Convolution Simulation: CTFConvolution Simulation: CTFTilt SeriesFocal & Tilt Series
Fourier Transform of the PSF0
0.2
0.4
0.6
0.8
1
-0.3 -0.2 -0.1 0 0.1 0.2 0.3
Focal&TiltTilt
Mag
nitu
de o
f Fou
rier
Com
pone
nt (a
.u.)
Ky (1/nm)
kz
ky
Peter Ercius, Cornell University
Depth ResolutionDepth Resolution
0
0.2
0.4
0.6
0.8
1
-1 -0.5 0 0.5 1
Focal&TiltTiltTF20 Tilt
Nor
mal
ized
Inte
nsity
(a.u
.)
Depth (nm)• Depth information from focal series does not add to depth resolution• Tomography resolution: experiment is 1-2nm (Why!?)
- Tomography yields 10x worse resolution in practiceAlignment, stage movement (low mag)
FWHM-Corrected
F&T: 1.4ÅTilt: 1.4Å
UncorrectedTilt: 2.5Å
Peter Ercius, Cornell University
Conclusions: Tomography & CorrectorsConclusions: Tomography & Correctors
• Electron Tomography• Quantitative measurements of 3D objects• Incoherent Bright Field (IBF) STEM
• high ρ*Z and t• Impact of Correctors
• Improved lateral and depth resolution • Focal and Tilt series
• necessary for corrected instruments• 3x fewer tilts needed Faster!
• Resolution limits• No considerable increase in resolution predicted• Tilt stage quality, alignment, blurring
Peter Ercius, Cornell University
Peter Ercius, Cornell University
Contrast Reversal with ThicknessContrast Reversal with Thickness
Cu via
• HAADF STEM• 0° tilt
Cu line
300nm
Cu via
Cu line
• HAADF STEM• 70° tilt
Peter Ercius, Cornell University
Cu lines: PlanviewCu lines: Planview
Peter Ercius, Cornell University
Increasing the Collector Angle (θc)Increasing the Collector Angle (θc)
1 2
3 430 nm
3 mr 10 mr
80 mr ADF
θc>>θobj
•No Phasecontrast
•No Diffractioncontrast
θc<<θobj•Phasecontrast
•Diffractioncontrast
θc≈θobj
•No Phasecontrast
•Diffractioncontrast
The incoherent BF image is the complement of the ADF image
Peter Ercius, Cornell University
Fourier ReconstructionFourier Reconstruction“A 2D projection of a object is equivalent to a 2D slice through the Fourier transform of that object at the angle of projection.”
High frequencies under sampled
Missing wedge of information
Object 1 projection:the ‘ray-integral’
2 projections
3 projections 10 projections 32 projections
Weighted backprojection: Backprojection can be made more accurate by restoring the correct distribution of the spatial frequencies using a weighting filter.
Peter Ercius, Cornell University
Tomographic ReconstructionTomographic Reconstruction
Under sampling Missing wedge
Features perpendicular with the tilt axis are distorted
Yields a blurred reconstruction
Peter Ercius, Cornell University
Z-contrast Simulation MethodZ-contrast Simulation Method
⊗ =
PSF39 depth slicesDepth: 5.1 Å/sliceLateral: .2 Å/pixel
( )zyx ,,δ
( )3Å100
z
x
y
Focal Series
20 depth slices∆f: 5 Å
3D incoherent Z-contrast STEM imaging simulation
Peter Ercius, Cornell University
Fourier Slice TheoryFourier Slice Theory
t
projection
θ
θ
F[f(x,y)]
Real space
ky
kx
Frequency space
Peter Ercius, Cornell University
Aberration CorrectorsAberration Correctors• Lens aberrations create phase shifts for e-’s
incident at different angles
• For given C-values…maximize α to maximize resolution– Including depth resolution ∆z
( )
281
61
41
212
max
87
65
43
2
πχ
ααααλπαχ
=
⎟⎠⎞
⎜⎝⎛ ++++∆−= LCCCf
2
22.1α
λ∝∆z
Peter Ercius, Cornell University
Balance Spherical Aberration Against Diffraction
Balance Spherical Aberration Against Diffraction
1
10
100
1 10
Prob
e Si
ze (A
ngst
rom
s)
α (mrad)
ds
d0
220
2stot ddd +≈
Optimal apertureAnd minimum
Spot size
• Balance sperical aberration against the aperture’s diffraction limit• Less diffraction with a large aperture – must be balanced against C3
• For a rough estimate of the optimum aperture size, convolve blurring terms• Add in quadrature:
Peter Ercius, Cornell University
Electron Lens Aberration CorrectorsElectron Lens Aberration Correctors
Design corrector to give no phase shift across the lensThere are other higher order aberrations that limit resolution
Lens aberrations are a power series that does not convergeYou can correct C3 but C5 limits you, correct C5 but C7 limits you, etc…