KIMIA ANALISIS INSTRUMEN II
Siska Ela Kartika, M.Si.
Topic
01 SEM Vs Microscope
Instrumentation and
02 principle of SEM
03 Sample preparation
Image formation in the
04 SEM
05 EDS
SEM
SEM (Scanning Electron
Microscope)
A type of microscope that
uses a focused beam of
electrons to scan a
surface of a sample to
create a high resolution
image and it produces
images that can show
information on a material’s
surface composition and
topography
SEM Vs Microscope
Items Microscope SEM
Source Light Electron beam
Resolution 0,1 m 0,1 nm
Usage Visual inspection with m level Visual analysis with nm level
Specialty 2D image inspection 3D image inspection
Preprocessing Need for same application Need some preprocessing and coating
Conditions Use in air Use in high vacuum
Magnification 5 – 1000 x 10 – 300.000 x
SEM Instrumentation
Principle of SEM
The electron gun produces an electron
beam
Electrons flowing into the anode
A magnetic lens is used for focusing
the electrons
Electrons strike the specimen and
produce a signal
The detector is used for detecting the
electrons emitted from the specimen
The computer displays an image
S A M P L E
PREPARATION
Conductivity requirement
The specimens examined by SEM must be able to withstand the strong
electric currents produced by the electron beam
Non-conductive sample
• The sample that does not conduct electricity can be damaged by the charges
that can build up
• Nonconductive specimens must first be coated with a thin layer of conductive
material
• A sputter coater coats the sample with gold
The purpose is to make non-metallic samples electrically conductive
Image formation in the SEM
Various signals emitted from the specimen when the electron beam strikes the specimen
SEM utilizes these signals to observe & analyze the specimen surface
Electron
beam
The translucent power of the electron
Low
beams in each sample is different Voltage
Material with
depending on the electron energy, the
a low atomic
atomic number, and the density of the number
atoms
High
Voltage
Higher energy has a deeper Electron
beam
distribution of electrons in the sample
Low
Volta
Material with ge
Large numbers of atoms and densities a high atomic
have a more limited distribution of number High Voltage
electrons
Secondary Electron (SE)
• Generated from a collision
between primary beam electrons
and loosely bonded outer
electrons
• Low energy electrons (10-50 eV)
• Only SE close to surface
escape: topographic information
obtained
• Number of SE is greater than the
number of incoming electrons
Backscattered Electron (BSE)
• Electrons (from the incoming
beam) are deflected by the
electrostatic field of a positive
nucleus
• Elastically scattered electrons:
don’t lose energy
• High-energy electrons (>50 eV)
• Able to escape from deeper in
the sample
SEM IMAGE
1000x magnification 3000x magnification
SE Vs BSE
Image maps a deeper region,
yield depends on the atomic
number of the specimen.
If different parts of the sample
consist of elements with
different atomic numbers then
the corresponding image parts
will have difference in
brightness
SE BSE
• SE show surface details & morphology • BSE show elemental differences due to the
differences density & atomic makeup of the sample areas
• Thin materials and small surface • Brighter areas are generally denser (higher
structures are evident with secondary atomic number) than darker areas
electron images.
Insect Pollen Aluminum Polymer Filter
Freezing technique
Cucumber Lung tissue
The advantages and
disadvantages of SEM
Advantages Disadvantages
Greater depth of field (focus depth) compared to Requires vacuum conditions
optical microscopy
Higher magnification Surface analysis only
Image dimension 3D The sample must be a conductive material,
otherwise it must be coated with metal
Lower resolution than TEM
Grey scale
SEM Vs TEM
SEM TEM
Electron stream Focused beam Broad beam
Image taken Topographical/surface Internal structure
Resolution Lower resolution (0.7 nm) Higher resolution (0.1 nm)
Magnification Up to 2,000,000 times Up to 50,000,000 times
Image dimension 3-D 2-D
Speed Faster Slower
Cost Less expensive More expensive
Operation Easy to use More complicated, requires training
Electron beam scanning An electron beam scans over the An electron beam passes through the
surface of the sample thin sample
Characteristic X-Ray
P r o d u c t i o n
Information on the
chemical composition
of the sample
• An inner shell electron is ejected by
an incoming electron (unstable)
• An outer shell electron drops down
to fill the vacancy (stable)
• The energy difference is emitted as
an X-ray photon
SEM-EDS
IMAGES
The Energy Dispersive
X-ray Spectrometer (EDS)
is used to analyze
characteristic X-ray
spectra by measuring the
energies of the X-rays
EDS Application
Material evaluation & identification
Contaminants
Failure analysis
• Contamination identification
Quality control screening • Unknown identification
Material verification
Plating specification &
certification