Partha Pratim Chowdhury

Postdoctoral Researcher

Department of Chemical Engineering

PI: Prof. Sheena Reeves

1
 Transmission Electron Microscopy (TEM)
• The wave nature of electron is used in TEM

• Accelerated electron beam in vacuum (~10-5 mm of Hg) from electron gun (generally
tungsten/LaB6/CeB6 wire) is the light source as compared to visible light in the optical microscope

• The resolution achieved is much higher than visible light due to much higher energy of electron wave

• Useful to get 2D images and information of objects at nano level which is beyond resolution limit of
visible light (~200 nm). This includes morphology, internal structure and lattice structure.

• This wavelength of the electron beam can be calculated from de Broglie’s equation. The wavelength
is dependent on the accelerating voltage and the resolution on wavelength and geometry.

At 100 kV of accelerating
voltage, the resolution will be 2
around 0.004 nm
Electron beam interaction with the sample

3
 Schematics

All the lenses here are

electromagnetic in nature,
except the anode used for
the electron gun which is
electrostatic in nature

4
Sample holder and carbon coated copper grid

5
 TEM Images (bright field images)

TEM image of Colloidal

nanoparticles. Drop casted on the
carbon coated copper grid. Very
useful to determine shape and
size

Colloids and Surfaces A: Physicochem. Eng. Aspects 466 (2015) 189–196

ACS Biomater. Sci. Eng. 2019, 5, 6, 3111–3118

Here the electron beam un scattered are allowed to pass whereas

electron beam absorbed or scattered are excluded thus providing
the contrast

6
 Other modes of imaging

Dark field image Diffraction

Image produced only by scattered Occurs due to elastic interference of the
electrons (all un scattered electron beam as it passes through a crystalline
electrons are excluded). Helpful sample. This also provide insightful information
in studying crystal defects and about crystal structure and phases
crystallographic phases

J. Mater. Chem., 2010, 20, 1147–1155

H. Wu and X. Zhu, ‘Perovskite Oxide Nanocrystals — Synthesis,
Characterization, Functionalization, and Novel Applications’, Perovskite
Materials - Synthesis, Characterization, Properties, and Applications. 7
InTech, Feb. 03, 2016. doi: 10.5772/61640.
 Aberrations
Spherical aberration

Caused by the lens field acting in

homogeneously on the off-axis rays. The rays
that are 'parallel' to the optic axis but at
different distances from the optic axis fail to
converge at the same point. The further off-axis
the electron is, the more strongly it is bent back
toward the axis

Chromatic aberration

The term chromatic aberration is related to

the energy of the electrons. Electrons are
not monochromatic. Electrons emerge from
the gun at a whole range of energies and
are bent by the objective lens to different
degrees; electrons that have lost energy are
bent more strongly

8
 Scanning Electron Microscope (SEM)
• Basic principle is same as that of TEM

• It generally measures images from backscattered and secondary electrons

• Topography of the sample can be measured in 3-D appearance along elemental composition

• It generally has lower accelerating voltage and lower resolution (~1-2 nm) than TEM. It’s less costly

• It scans through the entire sample to generate signals unlike TEM where it illuminates a certain part of the
sample at a time

• Don’t need elaborate sample preparation and thickness does not matter

• It is smaller in size than TEM and provide image faster than TEM

• The information of sample that SEM gives is different from that of TEM

9
Schematic
Backscattered electrons

They originates after elastic scattering of electron beam from deep

inside the sample, and the number is directly proportional to the
atomic number. They can help to differentiate phases and provide
compositional information

Secondary electrons

They are the electrons emitted from the surface of the sample when
irradiated by electron beam and is a result of inelastic scattering. They
provide topographical information. They have lower energy than
backscattered electron

10
 SEM sample holders and preparation

• The two -sided carbon adhesive are put on the sample holder and then then sample is pasted on that

• If the sample is non-conductive (say insulator) like cellulose materials, gold coating on the sample is
done by sputtering
to prevent buildup of electrostatic charge

11
 SEM Images

High flux novel polymeric membrane for renal applications. Sci Rep 13, 11703 (2023)

https://www.gla.ac.uk/schools/ges/research/researchfacilities/isaac/services/scanningelectronmicroscopy/imaging/secondaryelectronseandbackscatteredelectronbse/
12
 Energy-dispersive X-ray spectroscopy (EDS)
• It is a microanalytical technique used for identification and quantification of elements in a sample

• The working unit comes with electron microscopy, SEM or TEM

• It works by measuring the energy of X-Ray emitted by the sample when hit by an electron beam

• When microscope's high-energy electron beam interacts with the atoms of the sample there is ejection of
an atom's inner-shell electron (generally K shell for Z<35) creating an electron vacancy, which is quickly
occupied by a higher-energy, outer-shell electron.

• As the outer-shell electron drops to a lower-level shell it loses energy, and this excess energy is emitted as
X-rays. This characteristic X-Ray energy is used to identify element which is directly proportional to atomic
number

Not effective for elements

with low atomic number

13
 Elemental Mapping and detection in EDS
• This technique is used to visualize and characterize the spatial distribution of elements within a sample

• It is done by combining the point-by-point information collected by EDS

• Here the intensity and color is directly related to the concentration of an element

• Higher intensity or brighter color represents higher concentration and vice versa

• Silicon drift detector (SDD) is generally used as detector. Here the X-Ray photon is converted to electron hole
pair. The no. of electron is proportional to X ray energy

EDX spectra (top) and

corresponding Elemental
mapping (bottom

EDS spectra of shrimp

Sensors 2020, 20(20), 5889

14
 Wavelength dispersive electron spectroscopy (WDS)

• It’s another X-Ray dispersion technique like EDS

• Here instead of energy dispersion , the focus is on wavelength dispersion

• It has higher resolution (~10 times) and lower detection limit than EDS.
Hence can be useful to detect trace elements

• It is generally a slower method as compared to EDS

• It is generally used in conjugation with electron probe micro

analyzers (EPMA)

• A crystal monochromator with a fixed lattice spacing is used for

detection of X Ray which is done based on wavelength (Braggs Law
to be satisfied) 15
 Nanogenerator
• It is a technology that uses nanomaterials for generating electricity

• This technology converts mechanical or maybe the thermal energy as produced by small scale
physical change into electricity

• Energy produced by this nanogenerator will be few nanowatts to several milliwatts

• Based on mechanism they can be classified into 5 categories

Nanogenerator

Electromagneti
Piezoelectric Triboelectric Pyroelectric Thermoelectric
c

16
 Pyroelectric nanogenerator
• It’s an energy harvesting device converting the external thermal energy (temporal temperature
change) into electrical energy by using nanostructured pyroelectric materials. Useful for
harvesting waste heat energy.

• For having pyroelectric effect, the material must have spontaneous polarization (dipole moment
per unit volume in absence of electric field), which occurs due to non symmetric crystal
structure

• When heated, the crystal structure changes, and a reduction in spontaneous polarization takes
place and they exhibit potential difference at both ends of materials

• When cooled the reverse effect takes place which again results in potential difference

17
Adv. Funct. Mater. 2024, 34, 2312245
Thank You!

18