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Scanning Electron Microscopy (SEM)
What is Scanning Electron Microscopy (SEM)
A typical SEM instrument, showing the electron column, sample chamber, EDS
detector, electronics console, and visual display monitors.
The Geoscience Department's former electron microscope and energy dispersive
x-ray spectrometer. (No longer functioning.)
The scanning electron microscope (SEM) uses a focused beam of highenergy electrons to generate a variety of signals at the surface of solid
specimens. The signals that derive from electron-sample interactions
reveal information about the sample including external morphology
(texture), chemical composition, and crystalline structure and orientation
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of materials making up the sample. In most applications, data are
collected over a selected area of the surface of the sample, and a 2dimensional image is generated that displays spatial variations in these
properties. Areas ranging from approximately 1 cm to 5 microns in width
can be imaged in a scanning mode using conventional SEM techniques
(magnification ranging from 20X to approximately 30,000X, spatial
resolution of 50 to 100 nm). The SEM is also capable of performing
analyses of selected point locations on the sample; this approach is
especially useful in qualitatively or semi-quantitatively determining
chemical compositions (using EDS), crystalline structure, and crystal
orientations (using EBSD). The design and function of the SEM is very
similar to the EPMA and considerable overlap in capabilities exists
between the two instruments.
SEM stands for scanning electron microscope. The SEM is a microscope
that uses electrons instead of light to form an image. Since their
development in the early 1950's, scanning electron microscopes have
developed new areas of study in the medical and physical science
communities. The SEM has allowed researchers to examine a much
bigger variety of specimens.
The scanning electron microscope has many advantages over traditional
microscopes. The SEM has a large depth of field, which allows more of a
specimen to be in focus at one time. The SEM also has much higher
resolution, so closely spaced specimens can be magnified at much higher
levels. Because the SEM uses electromagnets rather than lenses, the
researcher has much more control in the degree of magnification. All of
these advantages, as well as the actual strikingly clear images, make the
scanning electron microscope one of the most useful instruments in
research today.
The SEM is an instrument that produces a largely magnified image by
using electrons instead of light to form an image. A beam of electrons is
produced at the top of the microscope by an electron gun. The electron
beam follows a vertical path through the microscope, which is held within
a vacuum. The beam travels through electromagnetic fields and lenses,
which focus the beam down toward the sample. Once the beam hits the
sample, electrons and X-rays are ejected from the sample.
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Diagram courtesy of Iowa State University
Detectors collect these X-rays, backscattered electrons, and secondary
electrons and convert them into a signal that is sent to a screen similar to
a television screen. This produces the final image.
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Fundamental Principles of Scanning Electron Microscopy
(SEM)
Accelerated electrons in an SEM carry significant amounts of kinetic
energy, and this energy is dissipated as a variety of signals produced by
electron-sample interactions when the incident electrons are decelerated
in the solid sample. These signals include secondary electrons (that
produce SEM images), backscattered electrons (BSE), diffracted
backscattered electrons (EBSD that are used to determine crystal
structures and orientations of minerals), photons (characteristic X-rays
that are used for elemental analysis and continuum X-rays), visible light
(cathodoluminescence--CL), and heat. Secondary electrons and
backscattered electrons are commonly used for imaging samples:
secondary electrons are most valuable for showing morphology and
topography on samples and backscattered electrons are most valuable for
illustrating contrasts in composition in multiphase samples (i.e. for rapid
phase discrimination). X-ray generation is produced by inelastic
collisions of the incident electrons with electrons in discrete ortitals
(shells) of atoms in the sample. As the excited electrons return to lower
energy states, they yield X-rays that are of a fixed wavelength (that is
related to the difference in energy levels of electrons in different shells
for a given element). Thus, characteristic X-rays are produced for each
element in a mineral that is "excited" by the electron beam. SEM analysis
is considered to be "non-destructive"; that is, x-rays generated by electron
interactions do not lead to volume loss of the sample, so it is possible to
analyze the same materials repeatedly.
How is a sample prepared?
Because the SEM utilizes vacuum conditions and uses electrons to form
an image, special preparations must be done to the sample. All water
must be removed from the samples because the water would vaporize in
the vacuum. All metals are conductive and require no preparation before
being used. All non-metals need to be made conductive by covering the
sample with a thin layer of conductive material. This is done by using a
device called a "sputter coater." . Most electrically insulating samples are
coated with a thin layer of conducting material, commonly carbon, gold,
or some other metal or alloy. The choice of material for conductive
coatings depends on the data to be acquired: carbon is most desirable if
elemental analysis is a priority, while metal coatings are most effective
for high resolution electron imaging applications. Alternatively, an
electrically insulating sample can be examined without a conductive
coating in an instrument capable of "low vacuum" operation.
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The sputter coater uses an electric field and argon gas. The sample is
placed in a small chamber that is at a vacuum. Argon gas and an electric
field cause an electron to be removed from the argon, making the atoms
positively charged. The argon ions then become attracted to a negatively
charged gold foil. The argon ions knock gold atoms from the surface of
the gold foil. These gold atoms fall and settle onto the surface of the
sample producing a thin gold coating.
What are the radiation safety concerns?
The radiation safety concerns are related to the electrons that are
backscattered from the sample, as well as X-rays produced in the process.
Most SEMs are extremely well shielded and do not produce exposure
rates greater than background. However, scanning electron microscopes
are radiation-generating devices and should be at least inventoried. The
Indiana State Department of Health requires that the machines be
registered with their office using State Form 16866, Radiation Machine
Registration Application. It is also important that the integrity of the
shielding is maintained, that all existing interlocks are functioning, and
that workers are aware of radiation safety considerations.
Strengths and Limitations of (SEM)? Strengths
There is arguably no other instrument with the breadth of applications in
the study of solid materials that compares with the SEM. The SEM is
critical in all fields that require characterization of solid materials. While
this contribution is most concerned with geological applications, it is
important to note that these applications are a very small subset of the
scientific and industrial applications that exist for this instrumentation.
Most SEM's are comparatively easy to operate, with user-friendly
"intuitive" interfaces. Many applications require minimal sample
preparation. For many applications, data acquisition is rapid (less than 5
minutes/image for SEI, BSE, spot EDS analyses.) Modern SEMs generate
data in digital formats, which are highly portable.
Limitations
Samples must be solid and they must fit into the microscope chamber.
Maximum size in horizontal dimensions is usually on the order of 10 cm,
vertical dimensions are generally much more limited and rarely exceed 40
mm. For most instruments samples must be stable in a vacuum on the
order of 10-5 - 10-6 torr. Samples likely to outgas at low pressures (rocks
saturated with hydrocarbons, "wet" samples such as coal, organic
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materials or swelling clays, and samples likely to decrepitate at low
pressure) are unsuitable for examination in conventional SEM's.
However, "low vacuum" and "environmental" SEMs also exist, and many
of these types of samples can be successfully examined in these
specialized instruments. EDS detectors on SEM's cannot detect very light
elements (H, He, and Li), and many instruments cannot detect elements
with atomic numbers less than 11 (Na). Most SEMs use a solid state x-ray
detector (EDS), and while these detectors are very fast and easy to utilize,
they have relatively poor energy resolution and sensitivity to elements
present in low abundances when compared to wavelength dispersive xray detectors (WDS) on most electron probe microanalyzers (EPMA). An
electrically conductive coating must be applied to electrically insulating
samples for study in conventional SEM's, unless the instrument is capable
of operation in a low vacuum mode.
The main reasons for developing a SEM safety plan are:
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to keep accurate inventory of all SEM's on campus
(manufacturer/model, serial number, location, contact person and
phone number)
to warn workers of the risk of interfering with any safety devices
(investigator needs to have permission to override any interlocks or
warning devices)
to make sure shielding is not compromised (exposure rate not
greater than 0.5 mrem/hr at 5 cm from any surface of machine)
to let workers know who to contact in an emergency or if they have
any questions
Scanning Electron Microscope Radiation Safety Guidelines
1. Safety evaluations will be performed initially when machine is
purchased and after machine has been moved.
2. Each machine should be key controlled when not in use. Interlocks,
if present, must remain operational unless approved by the RSO.
3. Shielding must be sufficient to maintain exposure rates less than
0.5 mrem/hr at 5 cm.
4. The Radiation Safety Office will keep inventory and survey
information on file in their offices. The SEM user should keep
logbook of any maintenance done on machine. RSO must be
notified if any modifications are made to the interlocks or any other
safety devices. The SEM user should also keep a copy of operating
and emergency procedures at the accelerator panel.
5. No survey meters or personnel dosimetry are required.