Course code-MEO 406

Unit-III. CHARACTERIZATION
Lecture-12

Kishor Upadhyaya
upadhyayakishor@gmail.com
9902047144
 Characterizing?? Looking at the characteristics or properties

Why needed??
Understand
Apply

How??
Probe
Study the responses
 Mechanical-Indentation, AFM Morphology-Microscope

Electrical- Hall measurement Properties Structure-XRD and TEM

Composition-EDAX,XPS Optical-PL, UV-Vis-IR, Raman

 Morphology-Microscopy

Limitations of optical microscopes:

Low magnification and resolutions
They cannot observe internal structures of micro elements
Light wavelength dependent.

High Resolution Microscopes

Electron Microscope Probe Microscope

SEM, TEM AFM, STM
 Electron Microscope
Uses an electron beam to illuminate a specimen and produce a magnified image.

Ernest Ruska and Max Knoll in 1931

Reinhold Rudenberg, the scientific director of Siemens-Schuckertwerke,
obtained the patent for the electron microscope in May 1931.
In 1932, Ernst Lubcke of Siemens & Halske built and obtained images.
In 1937, Manfred von Ardenne pioneered the SEM.
The first practical electron microscope was constructed in 1938, at the
University of Toronto, by Eli Franklin Burton and students Cecil Hall, James
Hillier, and Albert Prebus.
Siemens produced the first commercial transmission electron microscope
(TEM) in 1939

Magnification- 2 million
Resolution- 50 pm
Ernst Ruska Electron Microscope - Deutsches Museum - Munich
 Transmission Electron Microscope

A beam of electrons is transmitted through an ultra-thin specimen,

interacting with the specimen as it passes through.
An image is formed from the interaction of the electrons transmitted
through the specimen.
The image is magnified and focused onto an imaging device, such as a
fluorescent screen, on a layer of photographic film, or to be detected by a
sensor such as a CCD camera.
 Transmission Electron Microscope
Components:

1. Electron gun: LaB6 200 300keV.

2. Electron lenses:
Converge and deviate the e-beam.
EM coils of iron, iron-cobalt or nickel cobalt alloys are used.
The condenser lenses are responsible for primary beam formation.
The objective lenses focus the beam that comes through the sample itself
The projector lenses are used to expand the beam onto the phosphor
screen or other imaging device, such as film.
3. Aperture: Metallic disc for permitting axial electrons.

The transmitted beam contains information about electron density, phase and periodicity;
this beam is used to form an image.
30 nm Polio virus Silica coated Au NPs

TITAN-FEI, JNCASR

3-D image can also be constructed !!

 Scanning Electron Microscope

Manfred von Ardenne in 1937

Produces images of a sample by scanning it with a

focused beam of electrons.

The electrons interact with atoms in the sample,

producing various signals that can be detected and
that contain information about the sample's surface
topography and composition.
The electron beam is generally scanned in a raster
scan pattern, and the beam's position is combined
with the detected signal to produce an image.
SEM can achieve resolution better than 1 nanometer.
 Scanning Electron Microscope

Principle and working:

The most common mode of detection is by secondary

electrons emitted by atoms excited by the electron beam.
The number of secondary electrons is a function of the angle
between the surface and the beam.
On a flat surface, the plume of secondary electrons is mostly
contained by the sample, but on a tilted surface, the plume is
partially exposed and more electrons are emitted.
By scanning the sample and detecting the secondary electrons,
an image displaying the tilt of the surface is created

Magnification-5 lakhs, Resolution-1nm

SEM
 Nanowall Network

Nanorods
Pollen grains

500 nm
 Scanning Probe Microscopy

Scanning probe microscopy (SPM) is a branch of microscopy that

forms images of surfaces using a physical probe that scans the
specimen.
SPM was founded with the invention of the scanning tunneling
microscope in 1981.
No vacuum required.
30 types!!

1. Scanning Tunneling Microscopy (STM) Atomic Resolution!

2. Atomic Force Microscopy (AFM) The ability of piezoelectric actuators to execute motions
with a precision and accuracy at the atomic level or better
on electronic command.
Piezoelectric techniques".

Tips are typically SiN or Pt/Ir and single atom terminated.

 Scanning Tunneling Microscopy

Invented in 1981 by Gerd Binnig and Heinrich Rohrer (at IBM Zrich) - Nobel Prize in Physics in 1986

0.1 nm lateral resolution and 0.01 nm depth resolution

Not only UHV but also in air, water, and various other liquid or gas ambient, and at temperatures ranging from near zero kelvin
to a few hundred degrees celsius

The STM is based on the concept of quantum tunneling.

The resulting tunneling current is a function of tip position,
applied voltage, and the local density of states (LDOS) of the
sample.
Information is acquired by monitoring the current as the tip's
position scans across the surface, and is usually displayed in
image form.

Requires extremely clean and stable surfaces, sharp tips,

excellent vibration control, and sophisticated electronics.
STM
 Atomic Force Microscopy

Binnig, Quate and Gerber invented the first AFM in 1986.

The first commercially available atomic force microscope was introduced in 1989.

When AFM tip is brought into proximity of a sample surface, forces between the tip
and the sample lead to a deflection of the cantilever according to Hooke's law.
Cantilever deflection depends on mechanical contact force, van der Waals forces,
capillary forces, chemical bonding, electrostatic forces, magnetic forces (MFM), etc.
This deflection is measured using a laser spot reflected from the top surface of the
cantilever into an array of photodiodes.
A feedback mechanism is employed to adjust the tip-to-sample distance to maintain a
constant force between the tip and the sample.
Traditionally the tip or sample is mounted on a 'tripod' of three piezo crystals, with each
responsible for scanning in the x,y and z directions

Contact or static
Modes
AFM
Dynamic (non-contact or "tapping")