Scanning Electron Microscopy (SEM)

Susan Swapp, University of Wyoming

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 scanning electron microscope (SEM) uses a focused beam of high-energy 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 of materials making up the sample. In most applications, data are collected
over a selected area of the surface of the sample, and a 2-dimensional 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.

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.

Scanning Electron Microscopy (SEM)

Instrumentation - How Does It Work?

Essential components of all SEMs include the following:

 Electron Source ("Gun")

 Electron Lenses

 Sample Stage

 Detectors for all signals of interest

 Display / Data output devices

 Infrastructure Requirements:

o Power Supply

o Vacuum System
o Cooling system

o Vibration-free floor

o Room free of ambient magnetic and electric fields

SEMs always have at least one detector (usually a secondary electron detector), and
most have additional detectors. The specific capabilities of a particular instrument are
critically dependent on which detectors it accommodates.

Applications

The SEM is routinely used to generate high-resolution images of shapes of objects (SEI)
and to show spatial variations in chemical compositions: 1) acquiring elemental maps or
spot chemical analyses using EDS, 2)discrimination of phases based on mean atomic
number (commonly related to relative density) using BSE, and 3) compositional maps
based on differences in trace element "activitors" (typically transition metal and Rare
Earth elements) using CL. The SEM is also widely used to identify phases based on
qualitative chemical analysis and/or crystalline structure. Precise measurement of very
small features and objects down to 50 nm in size is also accomplished using the SEM.
Backescattered electron images (BSE) can be used for rapid discrimination of phases in
multiphase samples. SEMs equipped with diffracted backscattered electron detectors
(EBSD) can be used to examine microfabric and crystallographic orientation in many
materials.

Strengths and Limitations of Scanning

Electron Microscopy (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
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 x-ray 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.

User's Guide - Sample Collection and

Preparation
Sample preparation can be minimal or elaborate for SEM analysis, depending on the
nature of the samples and the data required. Minimal preparation includes acquisition
of a sample that will fit into the SEM chamber and some accommodation to prevent
charge build-up on electrically insulating samples. 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.

Data Collection, Results and Presentation

Representative SEM images of asbestiform minerals from the USGS Denver Microbeam
Laboratory

UICC Asbestos Chrysotile 'A' standard

Tremolite asbestos, Death Valley, California

Anthophyllite asbestos, Georgia

Winchite-richterite asbestos, Libby, Montana

Literature
The following literature can be used to further explore Scanning Electron Microscopy
(SEM)

 Goldstein, J. (2003) Scanning electron microscopy and x-ray microanalysis. Kluwer

Adacemic/Plenum Pulbishers, 689 p.

 Reimer, L. (1998) Scanning electron microscopy : physics of image formation and

microanalysis. Springer, 527 p.

 Egerton, R. F. (2005) Physical principles of electron microscopy : an introduction

to TEM, SEM, and AEM. Springer, 202.
 Clarke, A. R. (2002) Microscopy techniques for materials science. CRC Press
(electronic resource)
http://serc.carleton.edu/research_education/geochemsheets/techniques/SEM.html
 Scanning Electron Microscope
Advantages and Disadvantages in
ImagingComponents and Applications
A Scanning Electron Microscope (SEM) is a powerful magnification tool that utilizes
focused beams of electrons to obtain information.

The high-resolution, three-dimensional images produced by SEMs provide topographical,

morphological and compositional information makes them invaluable in a variety of
science and industry applications.

SEM Properties

The Scanning Electron Microscope developed by professor Dr. Charles Oatlev with the
assistance of graduate students in the 1950s, are one of the three types of electron
microscopes (EM).

Electron microscopes utilize the same basic principles as light microscopes, but focus
beams of energetic electrons rather than photons, to magnify an object.

SEMs consist of the following components:

 Electron Source
 Thermionic Gun
 Field Emission Gun
 Electromagnetic and/or Electrostatic Lenses
 Vacuum chamber
 Sample chamber and stage
 Computer
 Detectors (one or more)
 Secondary Electron Detector (SED)
 Backscatter Detector
 Diffracted Backscatter Detector (EBSD)
 X-ray Detector (EDS)
In addition, SEMs require a stable power supply, vacuum and cooling system, vibration-
free space and need to be housed in an area that isolates the instrument from ambient
magnetic and electric fields.

SEM Imaging

A Scanning Electron Microscope provides details surface information by tracing a sample

in a raster pattern with an electron beam.

The process begins with an electron gun generating a beam of energetic electrons down
the column and onto a series of electromagnetic lenses. SATU

These lenses are tubes, wrapped in coil and referred to as solenoids.

The coils are adjusted to focus the incident electron beam onto the sample; these
adjustments cause fluctuations in the voltage, increasing/decreasing the speed in which
the electrons come in contact with the specimen surface. DUA

Controlled via computer, the SEM operator can adjust the beam to control magnification
as well as determine the surface area to be scanned. TIGA

The beam is focused onto the stage, where a solid sample is placed. Most samples
require some preparation before being placed in the vacuum chamber.

Of the variety of different preparation processes, the two most commonly used prior to
SEM analysis are sputter coating for non-conductive samples and dehydration of most
biological specimens.

In addition, all samples need to be able to handle the low pressure inside the vacuum
chamber.

The interaction between the incident electrons and the surface of the sample is
determined by the acceleration rate of incident electrons, which carry significant
amounts of kinetic energy before focused onto the sample.

When the incident electrons come in contact with the sample, energetic electrons are
released from the surface of the sample. The scatter patterns made by the interaction
yields information on size, shape, texture and composition of the sample.

A variety of detectors are used to attract different types of scattered electrons, including
secondary and backscattered electrons as well as x-rays.

Backscatter electrons are incidental electrons reflected backwards; images provide

composition data related to element and compound detection. Although topographic
information can be obtained using a backscatter detector, it is not as accurate as an
SED.

Diffracted backscatter electrons determine crystalline structures as well as the

orientation of minerals and micro-fabrics.

X-rays, emitted from beneath the sample surface, can provide element and mineral
information.
SEM produces black and white, three-dimensional images.

Image magnification can be up to 10 nanometers and, although it is not as powerful as

its TEM counterpart, the intense interactions that take place on the surface of the
specimen provide a greater depth of view, higher-resolution and, ultimately, a more
detailed surface picture.

SEM Applications

SEMs have a variety of applications in a number of scientific and industry-related fields,

especially where characterizations of solid materials is beneficial.

In addition to topographical, morphological and compositional information, a Scanning

Electron Microscope can detect and analyze surface fractures, provide information in
microstructures, examine surface contaminations, reveal spatial variations in chemical
compositions, provide qualitative chemical analyses and identify crystalline structures.

SEMs can be as essential research tool in fields such as life science, biology, gemology,
medical and forensic science, metallurgy.

In addition, SEMs have practical industrial and technological applications such as

semiconductor inspection, production line of miniscule products and assembly of
microchips for computers.

SEM Advantages

Advantages of a Scanning Electron Microscope include its wide-array of applications, the

detailed three-dimensional and topographical imaging and the versatile information
garnered from different detectors.

SEMs are also easy to operate with the proper training and advances in computer
technology and associated software make operation user-friendly.

This instrument works fast, often completing SEI, BSE and EDS analyses in less than five
minutes. In addition, the technological advances in modern SEMs allow for the
generation of data in digital form.
 Although all samples must be prepared before placed in the vacuum chamber, most SEM
samples require minimal preparation actions.

SEM Disadvantages

The disadvantages of a Scanning Electron Microscope start with the size and cost.

SEMs are expensive, large and must be housed in an area free of any possible electric,
magnetic or vibration interference.

Maintenance involves keeping a steady voltage, currents to electromagnetic coils and

circulation of cool water.

Special training is required to operate an SEM as well as prepare samples.

The preparation of samples can result in artifacts. The negative impact can be minimized
with knowledgeable experience researchers being able to identify artifacts from actual
data as well as preparation skill. There is no absolute way to eliminate or identify all
potential artifacts.

In addition, SEMs are limited to solid, inorganic samples small enough to fit inside the
vacuum chamber that can handle moderate vacuum pressure.

Finally, SEMs carry a small risk of radiation exposure associated with the electrons that
scatter from beneath the sample surface.

The sample chamber is designed to prevent any electrical and magnetic interference,
which should eliminate the chance of radiation escaping the chamber. Even though the
risk is minimal, SEM operators and researchers are advised to observe safety
precautions.

Hitachi's Scanning Electron Microscope

Hitachi High-Technologies, formed in 2001, manufactures a variety of science and

technology related products.

Some Hitachi products include spectrophotometers, a variety of analyzers, inspection

equipment, electronic devices, and semiconductor products as well as a line of
microscopes.

They currently manufacture three scanning electron microscope models:

 S-3700N, an analytical style SEM ideal for studying large, heavy and tall samples
 S-3400N, a user-friendly, more compact model that utilizes new technology in electron
optics
 SU1510, a compact, high performance SEM that can handle large samples and
provides high-resolution imaging
http://www.microscopemaster.com/scanning-electron-microscope.html