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FYS 4340/9340 course – Autumn 2016 1
Diffraction Methods & Electron Microscopy
Sandeep Gorantla
FYS 4340/FYS 9340
Lecture 2
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FYS 4340/9340 course – Autumn 2016 2
Transmission Electron Microscopy
Sandeep Gorantla
Introduction and Basics Part- 1
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Learning more about TEM!
Courtesy: WWW.amazon.com
3 FYS 4340/9340 course – Autumn 2016
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Learning more about TEM!
4
http://www.matter.org.uk/tem/
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Learning more about TEM!
5
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FYS 4340/9340 course – Autumn 2016 6
Why learn about Transmission Electron Microscopy (TEM)?
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FYS 4340/9340 course – Autumn 2016 7
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FYS 4340/9340 course – Autumn 2016 8
Role of TEM in Materials Science Research and Development
Materials Science Paradigm
Courtesy: www.wikipedia.com
Solving Materials Science problems/mysteries by probing analytically and understanding structure-property relationships at atomic scale level
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FYS 4340/9340 course – Autumn 2016 9
graphite
graphene
nanotube fullerene
(Courtesy: The Royal Swedish Academy of Sciences)
Allotropes of carbon
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10
Courtesy: www.extremetech.com
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11
Courtesy: Knut Urban, Nature Materials 10, 165–166 (2011)
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1D nanomaterials modification in TEM
- Irradiation of solids with energetic particles usually leads to damage
- However, in the case of carbon nanostructures, electron irradiation was observed to have some beneficial effects
(a) Irradiation – mediated engineering
(b) self-assembly or self-organization
12
Courtesy: Krasheninnikov, A. V. et al., Nature Mater., 6, 723 (2007)
FYS 4340/9340 course – Autumn 2016
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FYS 4340/9340 course – Autumn 2016 13
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FYS 4340/9340 course – Autumn 2016 14
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FYS 4340/9340 course – Autumn 2016 15
Interface: defects on outer-wall of a nanotube and fullerene
Courtesy: Gorantla, S. et al., Nanoscale, 2, 2077 (2010)
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FYS 4340/9340 course – Autumn 2016 16
Courtesy: Gorantla, S. et al., Nanoscale, 2, 2077 (2010)
Movie Settings:
•Frame speed: 0.6 s •Total Frames: 48
Experimental conditions:
•Acquisition time: 1 s •Time gap between individual frames: 1s - 30s •Total time: 14 mins
Interface: defects on outer-wall of a nanotube and fullerene
Nanohump formation (Covalent interactions of fullerene fusion)
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FYS 4340/9340 course – Autumn 2016 17
Interface: defects on the outer-wall of a SWCNT and fullerene
Fullerene fusion with a nanohump (Covalent interactions of fullerene fusion)
Movie Settings:
•Frame speed: 0.6 s •Total Frames: 48
Experimental conditions:
•Acquisition time: 1 s •Time gap between individual frames: 1 s
Courtesy: Gorantla, S. et al., Nanoscale, 2, 2077 (2010)
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HETEROSOLAR PROJECT The aim of the work
Develop new solar cell devices base on
ZnO/Cu2O heterojunctions coupled with
convetional Si based solar cells
Si
* Theoretical eficiency ~20 %
* Highest exp. eficiency 1-4 %
ZnO Cu2O
Properties determined by the structures, faults
and interfaces.
n-type
3.4 eV 2.17 eV
p-type
TCO
Sub project : (S)TEM to characterize the thin films and their interfaces. 18
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FYS 4340/9340 course – Autumn 2016 19
ZnO
Cu2O
???
ZnO
Cu2O
50 nm
1 nm
ZnO Single Crystal
Cu2O (sputtering, 300nm)
CuO
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FYS 4340/9340 course – Autumn 2016 20
ZnO
CuO
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FYS 4340/9340 course – Autumn 2016 21
Transmission Electron Microscope Brief History
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Brief History: The first electron microscope
• Knoll and Ruska, first TEM in 1931
• Idea and first images published in 1932
• By 1933 they had produced a TEM
with two magnetic lenses which gave
12 000 times magnification.
Ernst Ruska: Nobel Prize in physics 1986
Electron Microscope Deutsches
Museum, 1933 model
22
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Brief History: The state-of-art TEM
Electron Microscope Deutsches
Museum, 1933 model
23
FEI Titan 60-300 TEM, NORTEM facility- UiO
Installed: 2014
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FYS 4340/9340 course – Autumn 2016
Resolution limit Year Resolution
1940s ~10nm
1950s ~0.5-2nm
1960s 0.3nm (transmission)
~15-20nm (scanning)
1970s 0.2nm (transmission)
7nm (standard scanning)
1980s 0.15nm (transmission)
5nm (scanning at 1kV)
1990s 0.1nm (transmission)
3nm (scanning at 1kV)
2000s <0.1 nm (Cs correctors)
Courtesy: http://www.sfc.fr/Material/hrst.mit.edu/hrs/materials/public/ElecMicr.htm
24
Brief History: The state-of-art TEM BIG LEAP: Introduction of Lens Aberration Correctors allowing atomic resolution at low accelerating voltages.
Core of the M100 galaxy seen through
Hubble (source: NASA)
Before Cs correction
After Cs correction
300 kV
200 kV
80 kV
60 kV
Typical TEM operating voltages
in Materials Science Research
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FYS 4340/9340 course – Autumn 2016 25
Transmission Electron Microscope Fundamentals
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Electrons interaction with the specimen
26
300 kV
200 kV
80 kV
60 kV
Typical TEM operating voltages
in Materials Science Research
Courtesy: D.B. Williams & C.B. Carter, Transmission electron microscopy
Electrons have both wave and particle nature
Typical specimen thickness
~ 100 nm or less
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Electron lenses
• Electrostatic – Not used as imaging lenses, but are used in modern monochromators
• ElectroMagnetic
– Can be made more accurately
– Shorter focal length
F= -eE
F= -e(v x B)
Any axially symmetrical electric or magnetic field have the properties
of an ideal lens for paraxial rays of charged particles.
Courtesy: http://www.matter.org.uk/tem/lenses/electromagnetic_lenses.htm
27 FYS 4340/9340 course – Autumn 2016
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TEM Lens Aberrations
• Spherical aberration coefficient
ds = 0.5MCsα3
M: magnification
Cs :Spherical aberration coefficient
α: angular aperture/
angular deviation from optical axis
r1
r2
Disk of least confusion
α
v
v - Δv
y-focus
x-focus y
x
Spherical aberration
Chromatic aberration Astigmatism
28 FYS 4340/9340 course – Autumn 2016
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TEM Lens Aberrations
29
Schematic of spherical aberration correction
Courtesy: Knut W. Urban, Science 321, 506, 2008; CEOS gmbh, Germany; www.globalsino.com
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TEM Lens Aberrations
Why we need an aberration-corrected TEM at 80kV???
-Correcting aberrations improves the TEM resolution at 80 kV
Uncorrected 80 kV ~ 0.3 nm
Corrected 80 kV ~ 0.14 nm
- Improved resolution enables the possibility of imaging carbon nanostructures at atomic level
30
Uncorrected 80 kV
Aberr. corrected 80 kV
(Courtesy: NASA)
FYS 4340/9340 course – Autumn 2016
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Transmission Electron Microscope Instrumentation – Part 1
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FEG gun
Extraction Anode Gun lens
Monochromator
Monochromator Aperture
Accelerator
Gun Shift coils C1 aperture/mono energy slit C1 lens
C2 lens C2 aperture Condenser alignment coils
C3 lens C3 aperture Beam shift coils
Mini condenser lens Objective lens upper Specimen Stage Objective lens upper
Image Shift coils Objective aperture
Cs Corrector
SA Aperture
Diffraction lens
Intermediate lens
Projector 1 lens
Projector 2 lens HAADF detector
Viewing Chamber Phosphorous Screen BF/CCD detectors
GIF CCD detector EELS prism
Courtesy: David Rassouw, CCEM, Canada
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Electron gun
Illumination system
Imaging system
Projection and Detection system
Specimen stage
Courtesy: David Rassouw
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FEG Electron gun source
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Specimen Stage
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TEM Specimen Holder
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TEM Specimens
• Typically 3 mm in diameter
Courtesy: http://asummerinscience.blogspot.no
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TEM Viewing Chamber – Phosphorous Screen
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TEM Image recording CCDs and EELS Spectrometer
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FYS 4340/9340 course – Autumn 2016 40
Transmission Electron Microscopy
Introduction and Basics Part-2
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TEM in Materials Science
The interesting objects for TEM is not the average structure or homogenous materials but
local structure and inhomogeneities
Defects
Precipitates
Interfaces
41
Atomic Structure Chemical bonding
Electronic Structure
Chemical composition
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FYS 4340/9340 course – Autumn 2016 42
Imaging Conventional TEM Bright/Dark-Field TEM High Resolution TEM (HRTEM) Scanning TEM (STEM) Energy Filtered TEM (EFTEM)
Diffraction Selected Area Electron Diffraction Convergent Beam Electron Diffraction
Spectroscopy
Electron Dispersive X-ray Spectroscopy (EDS) Electron Energy Loss Spectroscopy (EELS)
TEM techniques
Main Constrast phenomena in TEM •Mass thickness Contrast •Diffraction contrast •Phase Contrast •Z-contrast
Chemical composition, electronic states, nature of chemical bonding (EDS and EELS). Spatial and energy resolution down to the atomic level and ~0.1 eV.
Phase identification, defects, orientation relationship between different phases, nature of crystal structure (amorphous, polycrystalline, single crystal)
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Objective aperture: Contrast enhancement
All electrons contributes to the image. A small aperture allows only electrons in the
central beam in the back focal plane to contribute
to the image. Intensity: Thickness and density
dependence
Mass-thickness contrast
Si Ag and Pb
glue (light elements)
hole
50 nm One grain seen along a
low index zone axis.
Diffraction contrast (Amplitude contrast)
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Imaging Conventional TEM Bright/Dark-Field TEM High Resolution TEM (HRTEM) Scanning TEM (STEM) Energy Filtered TEM (EFTEM)
Diffraction Selected Area Electron Diffraction Convergent Beam Electron Diffraction
Spectroscopy
Electron Dispersive Spectroscopy (EDS) Electron Energy Loss Spectroscopy (EELS)
TEM techniques
200 nm
Simplified ray diagram of conventional TEM
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Imaging
Courtesy: http://www.ifam.fraunhofer.de; I.MacLauren et al, International Materials Review, 59, 115 (2004)
Bright
Field ADF ADF
specimen
Incident E-beam
scattered E-beam
(α = 22 mrad)
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Imaging
TEM STEM
Mass thickness and diffraction contrast Mass thickness and Z- contrast
Gd-Hf-Co-Al quaternary alloys
Z Gd 64 Hf 72 Co 27 Al 13
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Imaging
HRTEM STEM
Phase contrast Z- contrast
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Raw HAADF-STEM, ABF-STEM and HRTEM image of Si in the [110] zone axis by
FEI Titan 60-300 with spatial resolutions of 0.8 Å for STEM and 2.0 Å for TEM.
1.36 Å
HAADF-STEM ABF-STEM HRTEM
Courtesy: Wei Zhan, Øystein Prytz, et al. (2015), SMN, UiO
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Electron Diffraction in TEM
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Simplified ray diagram
Objective lense
Diffraction plane
(back focal plane)
Image plane
Sample
Parallel incoming electron beam Si
a
b
c
Po
wd
erCell 2
.0
1,1 nm
3,8
Å
Objective aperture
Selected area
aperture
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Elastic scattered electrons Only the direction of v is changing.
(Bragg scattering)
Elastic scattering is due to Coulomb interaction
between the incident electrons and the electric
charge of the electron clouds and the nucleus.
(Rutherford scattering).
The elastic scattering is due to the average
position of the atoms in the lattice.
Reflections satisfying Braggs law:
2dsinθ=nλ
Inelastic scattered electrons Direction and magnitude of v change.
Energy is transferred to electrons and atoms
in the sample.
-It is due to the movements of the atoms
around their average position in the lattice.
- It give rise to a diffuse background in the
diffraction patterns.
Electrons interacts 100-1000 times stronger with matter than X-rays -more absorption (need thin samples)
-can detect weak reflections not observed with XRD technique
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Electron Diffraction in TEM
Courtesy: Dr. Jürgen Thomas, IFW-Dresden, Germany
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Selected area diffraction(SAD)
• Parallel incoming electron beam and a selection aperture in the image plane.
• Diffraction from a single crystal in a polycrystalline sample if the SAD aperture is small enough/crystal large enough.
• Orientation relationships between grains or different phases can be determined.
• ~2% accuracy of lattice parameters
– Convergent electron beam better
Image plane
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Camera constant
R=L tan2θB ~ 2LsinθB
2dsinθB =λ
↓
R=Lλ/d
Camera constant:
K=λL
Film plate
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Indexing diffraction patterns
The g vector to a reflection is normal to the
corresponding (h k l) plane and IgI=1/dnh nk nl
- Measure Ri and the angles between
the reflections
- Calculate di , i=1,2,3 (=K/Ri)
- Compare with tabulated/theoretical
calculated d-values of possible phases
- Compare Ri/Rj with tabulated values for
cubic structure.
- g1,hkl+ g2,hkl=g3,hkl (vector sum must be ok)
- Perpendicular vectors: gi ● gj = 0
- Zone axis: gi x gj =[HKL]z
- All indexed g must satisfy: g ● [HKL]z=0
(h2k2l2)
Orientations of corresponding
planes in the real space
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Poly crystalline sample
The orientation relationship between the phases can be determined with ED.
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Single Crystals
Interface between two different phases
epitaxially grown
Electron Diffraction in TEM
Amorphous phase
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Spectroscopy
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FYS 4340/9340 course – Autumn 2016
Quartz (1mm)
AZO (sputtering, ~200 nm)
Cu2O (sputtering, 600nm)
TiO2 (ALD, 10 nm)
X-ray Energy Dispersive Spectroscopy
We detect the X-rays generated by the sample on a spectrometer Each element has a unique atomic structure and hence a characteristic X-ray energy
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FYS 4340/9340 course – Autumn 2016
Quartz (1mm)
AZO (sputtering, ~200 nm)
Cu2O (sputtering, 600nm)
TiO2 (ALD, 10 nm)
Energy Dispersive X-ray Spectroscopy
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Electron Energy Loss Spectroscopy (EELS)
Courtesy: William & Carter, Transmission Electron Microscopy; EM group, Univ. of Nevada, Reno.
Inelastically interacted incident electron suffers energy loss after passing through the specimen
• Phonon Excitations • Inter and Intraband Transitions • Plasmon Excitations • Inner Shell Ionizations • Cherenkov radiation
Each element has characteristic ionization energy owing to its unique atomic structure
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EELS of the Oxygen K edge The reference spectra of Cu2O and CuO are from online EELS database1. The reference spectra were shifted in energy to match the first O K peak in our experimental, and scaled by the total counts in the energy-loss 560-590 eV.
1Ngantcha, Gerland, Kihn & Riviere, Eur. Phys. J. Appl. Phys. 29, (2005) 83.
ZnO
CuO
Cu2O
Electron Energy Loss Spectroscopy (EELS)
Courtesy: Cecilie Granerod, SMN, UiO
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Next Lecture
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• TEM Instrumentation – Part 2 (Text book Chapters: 5 – 9)
• TEM Specimen Preparation
(Text book Chapters: 10)
FYS 4340/9340 course – Autumn 2016