Dharmapadmi P. K.

195160100111028

Scanning Electron Microscopy (SEM)

History of SEM
 In 1933, Electron Microscopy was invented by Ernst Ruska, a German
physicist. He was a
 Awarded the Nobel Prize for physics for his invention in 1986
 In 1938, First SEM debuted by Manfred Von Ardenne
 In 1965, Cambridge Scientific Instrument (UK) and JOEL (Japan) first
commercialized SEM individually

Introduction of SEM
The light microscope used photons while the electron microscope used
electrons. Photons are substituted with electrons and glass lenses are
substituted with electromagnetic and electrostatic lenses. The size of the light
microscope is more than 100nm (the size of a Mycoplasma) and less than 1mm
(the size of a frog egg). The size of an electron microscope is more than 0.1nm
(the size of atoms) and less than 100µm (the size of eukaryotic cells). Electron
microscopes are scientific instruments that use a beam of highly energetic
electrons to examine objects on a very fine scale.

Applications of SEM
 Topography is used to observe the surface features of the sample
 Morphology is used to observe the shape and size of the sample
 Composition is used to observe the elements that the sample is
composed of and their relative amount (%) – purity
 Crystallographic info is used to observe how atoms are arranged in the
sample
The SEM image shows a more detailed picture of the object than the
compound microscope image and TEM image. The TEM image shows a more
detailed image of the object than the Compound microscope image.

Instrumentation
The parts of SEM include:
 Electron cannon
 Electron gun consisting of a cathode and anode
 The condenser lens controls the number of electrons traveling down the
column
 The objective lens focuses the beam into a spot on the sample
 The deflection coil helps to deflect the electron beam
 SED attracts the secondary electrons
  Additional sensors detect backscattered electrons and x-rays
 Vacuum pumps system
 Operation panel with focus, alignment, and magnification tools and a
joystick for positioning
 Screen for menu and image display
 Cryo-unit to prepare frozen material before insertion in the observation
chamber in Cryo-SEM mode

Formation of an image
High-energy electrons shoot and the outgoing electron/x-rays analyze.
SEM changes the magnification of an image by reducing the size of the area
scanned by the scan coils. This form of image processing is only in gray. This
image can be colorized through the use of feature-detection software. This is
usually for aesthetic effects and adding a realistic effect.

Electron beam-sample interactions

The variety of products that are possible as a result of the interaction
between electrons and matter can be seen. All these varied types of signals
convey different beneficial information about the sample and it is the choice of
the microscope’s operator which signal to capture. For instance, in
transmission electron microscopy (TEM), as the name indicates, signals such
as the transmitted electrons are detected which will provide information on the
inner structure of the sample. In the case of a scanning electron microscope
(SEM), two types of signal are usually detected; the backscattered electrons
(BSE) and the secondary electron (SE).
Parameters on Electron beam-sample interactions are the incident
electron beam scattered in the sample, both elastically and inelastically. This
gives rise to various signals that we can detect. Interaction volume increases
with increasing acceleration voltage and decreases with increasing atomic
number.

Signals that can be used to characterize the microstructure

Backscattered electrons (BSE) are a fraction of the incident electrons that
are retarded by the electromagnetic field of the nucleus and if the scattering
angle is greater than 180 ° the electron can escape from the surface.
Backscattered electrons (BSE) consist of high-energy electrons originating in
the electron beam, that are reflected or back-scattered out of the specimen
interaction volume by elastic scattering interactions with specimen atoms.
Heavy elements (high atomic number) backscatter electrons more strongly than
light elements (low atomic number), and thus appear brighter in the image.
One of the signals that can be used to characterize the microstructure is
X-rays. Each element has a fingerprint X-ray signal. It has poorer spatial
resolution than BSE and SE. Relatively few X-ray signals are emitted and the
detector is inefficient (relatively long signal-collecting times are needed). The
most common spectrometer is EDS (energy-dispersive spectrometer). Signal
overlap can be a problem, so we can analyze our sample in different modes like
spot analysis, line scan, and chemical concentration map (elemental mapping).
Traditional guns or thermionic electron guns (electrons are emitted when
a solid is heated) ( with W-wire, LaB6-crystal). Modern or field emission guns
(FEG) (cold guns, a strong electric field is used to extract electrons) (with a
Single crystal of W, etched to a thin tip). Usually, we want many electrons per
time unit per area (high current density) and as small an electron spot as
possible. By using field emission guns (FEG) we can get a smaller spot and
higher current densities compared to thermionic guns, but we need a better
vacuum for a FEG.
There are 2 types of detectors, a Backscattered electron (BSE) detector
(Solid-State Detector) and a Secondary electron (SE) detector (Everhart-
Thornley). In traditional detectors. Traditional detectors, use those two
detectors and Energy dispersive spectrometer (EDS) as the X-rays.
The electron beam generated by the electron gun would encounter
interference from air particles in the atmosphere. These particles block the
path of the electron beam, they would also be knocked out of the air and onto
the specimen, which would distort the surface of the specimen. Vacuum
requirements are dependent on the type of detector. Chemical (corrosion) and
thermal stability are necessary for a well-functioning filament (gun pressure).
Charge-up is a phenomenon where the negative of the incident electron
beam accumulates (charged up) on the surface of a non-conductive specimen
and the potential in the beam-incident area changes to cause various image
troubles. The charge-up phenomenon occurs when the total number of
electrons emitted from a specimen, or backscattered electrons, absorbed
electrons, and secondary electrons is not equal to the number of incident
electrons. Charge-up can be prevented by coating the non-conductor sample
with metal (conductor), allowing the charge on the sample surface to go to the
ground through the coated conductive film.

Energy Dispersive X-ray Microanalysis (EDX/EDS)

An EDX spectrum was collected at each point identified in the top
secondary electron image to individually characterize the wires. The resulting
spectra show that the larger diameter wire is Ni, the medium diameter wire is
Al, and the thinnest diameter wire is Ti. A small amount of Ai smeared onto the
other wire surfaces when wires were wound together.

Resolution
  Best resolution that can be obtained size of the electron spot on the
surface of the sample
 The introduction of FEG has dramatically improved the resolution
of SEMs
 The volume from which the signal electrons are formed defines the
resolution
 SE image has a higher resolution than a BSE image
 Scanning speed :
 A weak signal requires slow speed to improve the signal-to-noise
ratio
 When doing a slow scan drift in the electron beam can affect the
accuracy of the analysis

Sample preparation
1. Coating specimen
A coating specimen is used to increase the conductivity of the specimen
and to prevent the high voltage charge on the specimen. All metals are
conductive and require no preparation before being used. Meanwhile,
non-metals need to be made conductive by using a device called a
"sputter coater". These non-metals will coat with thin layers i.e. 20nm –
30nm of conductive metal such as gold, gold-palladium alloy, platinum,
osmium, iridium, tungsten, chromium, and graphite. Appropriate size
sample that fits in the specimen chamber. Mounted rigidly on a
specimen holder in specimen stub. For imaging in the SEM, specimens
must be electrically conductive and electrically grounded.
2. Cleaning the surface of the specimen
Cleaning the specimen surface is very important because the surface
contains a lot of unwanted deposits, such as dust, mud, soil, etc.
3. Dehydrating the specimen
Dehydration of the specimen using water must be removed, air drying
causes collapse and shrinkage, this is usually achieved by replacing the
water in the cell with an organic solvent such as ethanol or acetone,
dehydration is carried out with a graded sequence of ethanol or acetone.
4. Drying the specimen
Dry the specimen by ensuring that the specimen is completely dry.
Otherwise, the sample will be destroyed.
5. Mounting the specimen
Furthermore, the way to place the specimen is that the specimen must
be mounted on a holder, rigidly mounted on specimen holder called a
specimen stub. For dry specimens, it is attached to the specimen stub
using an adhesive such as epoxy resin or electrically conductive double-
sided adhesive tape.
SEM Advantage
 Gives detailed 3D and topographical imaging and versatile information
garnered from different detectors.
 Works very fast.
 Modern SEMs allow for the generation of data in digital form.
 Most SEM samples require minimal preparation actions.

SEM Disadvantage
 SEMs are expensive and large.
 Special training is required to operate an SEM.
 The preparation of samples can result in artifacts.
 Limited to solid samples.
 Carry a small risk of radiation exposure associated with the electrons
that scatter from beneath the sample surface.

Environmental SEM (ESEM)

Traditional SEM chamber pressure is about 10-6Torr while ESEM is
0.08–30Torr. Various gases can be used by ESEM, and also requires different
SE detectors. The reason for using ESEM is to image challenging samples such
as insulating samples, vacuum (sensitive samples), irradiation (sensitive
samples), and wet samples. Also, ESEM is to study and image chemical and
physical processes in situ such as mechanical stress (testing), oxidation of
metals, and hydration or dehydration.

The use of FESEM in dentistry

An example of the use of FESEM in dentistry can be used to look at a
human tooth showing numerous dentin tubules X 900. It can be used to know
the demineralization using etching with 37% phosphoric acid for 15 seconds
and 10% sodium hypochlorite for 1 minute.
Epitaxial growth such as enamel is made up of tightly bunched, oblong
crystals that are about 1000 times smaller in width than human hair. Usually,
we need more than one analysis/ data to better support our findings. Example:
The use of various analyses in dentistry such as FESEM + XRD + HRTEM.
The XRD Spectra indicated the evolution process from CPICs to HAP on
the enamel window. SEM image showing both acid-etched enamel and repaired
enamel. TEM image showing the longitudinal section of the reconstructed layer
on natural enamel, including the native and repaired zone.
It has been applied to research such as the Synthesis of ZnO using
Bacillus cereus as the bio-templating agent (biomaterial as nanoreactor) and
Zinc oxide synthesized using diethylene glycol-hydrothermal method showing
carnation-like nanostructure.

Summary
 SEM is a versatile instrument for many applications, especially for the
study of surface morphology.
 To get a micrograph, an electron probe is scanned across the surface of
the samples and detectors interpret the signal as a function of time
 A resolution of 1-2nm can be obtained when operated in a high-
resolution setup.
 The introduction of ESEM and the field emission gun have simplified the
imaging of challenging samples
 Signals:
 Secondary electrons (SE) are mainly topography
 Backscattered electrons (BSE) are mainly chemistry
 X-rays (EDX) is chemistry