MSE 510 – Microstructural Characterization

Techniques - Lecture 21
• Virtual office hours M,W,F – Carlos Mon and Wed; Prof. Okuniewski
Fri
• Presentation to help with Final Presentation – posted on BB in Final
Project Folder
• Pandemic pick-me-up
• New sample preparation method published yesterday (!) for SEM and
TEM
• Introduction to TEM
• TEM Imaging and diffraction
• TEM Contrast mechanisms
Apr. 9, 2020 1
A little help from our furry friends …
A little help from our furry friends …

https://youtu.be/noL37SATDEw https://youtu.be/5l-7MYq1SOE?t=704
 New sample preparation method published
yesterday (!) for SEM and TEM

Nature Commun. 11(2020)1743.

Nature Commun. 11(2020)1743.
Nature Commun. 11(2020)1743.
TEM – General Comments - 1
TEM – General Comments - 2
 Advantages and Disadvantages of TEM
 Advantages
• Real (Image) and reciprocal space (diffraction pattern) information can be obtained from same region of sample.
• Chemical information via EDX and EELS possible (with additional attachments).
• Energy filtered images possible via EELS filter.
• High resolution imaging possible (via HRLFI & HAADF in STEM).
• Possible to obtain amplitude and phase contrast images.
• Many different kinds of phase contrast images can be obtained.

 Disadvantages
• Low sampling volume and rather slow process of obtaining information.
• Special training required for the operation of the equipment.
• Difficult sample preparation and possibility of electron beam damage.
• Samples which are not stable in vacuum are difficult to study.
• Magnetic samples require special care.
• Non-conducting samples require gold or carbon coating.
• Difficulty in the interpretation of images.

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https://www.iitk.ac.in/tkic/workshop/XRD/ppt/Prof%20Anandh/TEM.pdf
 Cross Section of a TEM

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https://nanohub.org/resources/3777 Ref: Transmission Electron Microscopy by William and Carter
 Types of interactions between thin specimen
and electron beam

• Transmitted electron (beam) TEM can acquire images,

• Diffracted electrons (beams) (Elastically scattered) diffraction patterns,
• Coherent beams spectroscopy and
• Incoherent beams chemically sensitive
• Inelastically scattered electrons images at sub-nanometer
• Characteristic X-rays to nanometer resolution.
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Ref: Transmission Electron Microscopy by William and Carter https://mrl.illinois.edu/sites/default/files/AMC/downloads/AMC-Workshop-2012_Tutorial-8_TEM.pdf
 What can we do with a TEM?
 Imaging
• Amplitude Contrast (Parallel Beam Illumination)
• Mass thickness contrast:
• Observe density changes in specimen
• Diffraction contrast (Bright Field and Dark Field):
• Dislocations, stacking fault, grain boundaries, precipitates and second phases
• Phase Contrast (Parallel Beam Illumination)
• HRTEM [Provides Fringes: Fringes in image = Spots in Diffraction images]
• Observe dislocations, stacking fault, grain boundaries, and precipitates
• Acquire Diffraction information by applying a Fourier Transform to image.
• STEM Imaging (Convergent Beam Illumination)
• Z-contrast imaging, Bright-field STEM imaging, High-resolution Z-contrast imaging (Bright- & Dark-field)
 Diffraction
• Selected Area Diffraction (Parallel Beam Illumination)
• Provide Crystal structure from selected areas of the specimen.
• Distinguishes and identify crystalline and amorphous regions of the phases.
• Convergent Beam Electron Diffraction (Convergent Beam Illumination)
• Point/space group and local strain determination.
 Spectroscopy (Convergent Beam Illumination)
• Energy Dispersive X-ray Spectroscopy
• Electron Energy Loss Spectroscopy
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 Types of illumination

Parallel Beam Illumination Focused Beam Illumination Translating/tilting the beam

• Provides illumination conditions • Provides illumination conditions • Provides illumination conditions
for imaging and diffraction. for structural and chemical for different quality of Bright
Eg: Mass Thickness contrast, information. Field and Dark Field imaging.
Diffraction Contrast, Phase contrast, Eg: STEM, EDS, EELS
diffraction.
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https://nanohub.org/resources/3777
 Diffraction and Imaging mode
TEM diffraction
• Reciprocal Space – Reciprocal Crystal
• Data represented in 1/r (r = units of length)
• Provides information on crystal structure,
periodicity, local strain.

TEM imaging
• Real Space – Crystal
• Data represented in r (r = units of length)
• Defects, and other phases can be observed

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https://nanohub.org/resources/3777
 What is Contrast?
• Contrast is quantitatively defined as the
difference in Intensity (ΔI) between two
adjacent areas:
𝐼2− 𝐼1
•𝐶= = ∆𝐼/𝐼1
𝐼1

Williams and Carter, Transmission Electron Microscopy, 1996.

2 Methods of Specimen Observation:
Imaging and Diffraction Patterns

Diffraction pattern

Forward scattered
beam directions

Image Diffraction Pattern

Diffraction Patterns
• Diffraction pattern:

Williams and Carter, Transmission Electron Microscopy, 1996.

Image

Williams and Carter, Transmission Electron Microscopy, 1996.

3 Primary Imaging Modes

Williams and Carter, Transmission Electron Microscopy, 1996.

3 Primary Imaging Modes

Williams and Carter, Transmission Electron Microscopy, 1996.

Bright Field Imaging

Okuniewski, PhD Dissertation,

University of Illinois, 2008.
Bright Field Imaging
Dark Field Imaging

Okuniewski, PhD Dissertation,

University of Illinois, 2008.
Dark Field Imaging
 HR-TEM

Williams and Carter, Transmission Electron Microscopy, 1996.

Major Imaging Contrast Mechanisms
 Mass-Thickness Contrast - 1

Fig 22.4

Williams and Carter, Transmission Electron Microscopy, 1996.

Mass-Thickness Contrast - 2

Fig 22.4
 Mass Thickness Contrast

Image Intensity
(a) TEM BF image of latex particles on a carbon support film
showing thickness contrast only. (b) Latex particles through the
addition of selective mass contrast to the image.
Mass Thickness Contrast
 Mass Thickness Contrast – Attenuation
Scattering Length for 1/e
material [1/e] thickness
C (Z=6) 200 nm
Ge (Z=32) 40 nm
Pt (Z=78) 9 nm

Williams and Carter, Transmission Electron Microscopy, 1996.

Mass Thickness Contrast – general comments
Mass Thickness Contrast – general comments