SCANNING ELECTRON MICROSCOPY

(SEM)
1. Introduction [1,2]:
A scanning electron microscope (SEM) is a type of electron microscope that produces
images of a sample by scanning it with a focused beam of electrons (fig. 1) [1].

Fig. 1 Scanning electron microscope (SEM)
In SEM, a fine probe of electrons with energies typically up to 40 keV is focused on a
specimen, and scanned along a pattern of parallel lines. Various signals are generated as a
result of the impact of the incident electrons, which are collected to form an image or to
analyze the sample surface. These are mainly secondary electrons, with energies of a few tens
of eV, high-energy electrons backscattered from the primary beam and characteristic X-rays
[2].
SEM can provide information on surface topography, crystalline structure, chemical
composition and electrical behavior of the top 1 m or so of specimen. Various specialized
stages (e.g. hot, cold or designed to permit in situ mechanical testing) can be attached to
enable behavior under various conditions to be examined [3].
Further advantages of SEM include [3]:
- SEM benefits from a large depth of field so most of the specimen surface is
simultaneously in focus whatever the surface roughness.
- SEM magnifications can be achieved (up to 1,000,000x), with an ultimate
resolution of 1 nm.
- The possibility of getting more information than just the surface topography, e.g.
crystal structure, chemical composition and electrical properties. Switching
between different imaging techniques enables information to be cross-correlated
with confidence.
- Large specimens (200 mm diameter wafers, or even larger in specially adapted
SEMs).
- SEM permits non-destructive evaluation of the specimen.
- Very short specimen preparation time (maybe only a few seconds) while the
specimen is attached to a stub (specimen holder).
2. History [4,5]:
The history of the electron - optical instruments traces back to three basic discoveries. In
1897 J. J. Thomsonl) proved the existence of the electron. In 1924 de Broglies) published his
hypothesis on the wave nature of material particles. In 1926 Buschs) showed that electric and
magnetic fields possessing axial symmetry acted as lenses on electrons and other charged
particles. These three steps initiated the development of a whole new science of
instrumentation called electron-optics. As stated previously, the development of the SEM and
he TEM began in the same decade.
In 1934 Ruska described a TEM. It was designed to surpass the resolution of the optical
light microscope (OLM). Five years later, Siemens and Halske, Germany, marketed a
production-line instrument capable of resolving 100.
In 1935 Knolls suggested the possibility of a SEM. Three years later, von Ardennes built
a SEM which utilized the transmitted current to obtain images (fig. 2). In 1942 Zworykin,
Hillier and Snyder achieved a resolution of 500 with their instrument. After the war, SEM
versions were constructed a new by Lecautes) and co-workers in France and a group under
Oatleyg) in England. The modifications made by the members of the latter group.

Fig. 2 M. von Ardenne's first SEM
3. The constructing principle of SEM [5]:
a. Principle
Fig. 3 illustrates the principle of the SEM. A finely-focused electron beam impinges on a
point in the specimen surface. The interaction between the electrons and the solid generates a
variety of signals. Each of these can be collected and amplified. The resulting signal is
utilized to control the brightness on a cathode ray tube (crt). To obtain signals from an area,
the electron beam is scanned in a TV-raster fashion over the specimen surface by two pairs of
electro-magnetic deflection coils. Because the crt scan is synchronized with the beam scan,
the signals are transferred point to point and a signal map of the scanned area is displayed.
Changes in brightness represent changes of a particular property within the scanned area of
the specimen. Operating parameters, such as accelerating voltage, beam diameter and current,
angle of incidence, and line and frame speeds are selected to optimize the quality of the
resulting image and to assure complete coverage of the crt.

Fig. 3 The principle of the SEM
b. Instrumentation
Fig. 4 shows the components of a SEM. The most common electron gun is a triode design.
A hair-pin shaped tungsten filament is usually the source of thermionic electrons. The current
and energy is determined by an adjustable negative potential on the bias and a positive
acceleration potential on the anode. This potential is usually variable between 1 and 50 kV.
A series of two or three electro-magnetic lenses is used to de-magnify the source diameter
to about 200 or less at the specimen. The final lens also contains the two sets of deflection
coils to allow the beam to be scanned in a square raster pattern. Apertures to define the
convergence of the beam and to reduce contamination of the lens surfaces, and a stigmator to
correct any system-induced astigmatism complete the electron-optical component.
To permit the scatter-free travel of the electrons from their source to the specimen (over
50 cm), a vacuum of less than 1 x 10m4 Torr has to be provided. This is achieved by a
combination of mechanical and oil diffusion pumps and a suitable valve arrangement.
Sacrificing time, clean ultra-high vacuum can be obtained by the use of ion, turbo-molecular
or cryogenic pumps.
Mechanical feed-throughs provide necessary specimen movement in the three dimensions
and rotation as well as tilt. For more complex specimen manipulations while under
observation, electrical feed-throughs are provided; heating, cooling and stress stages are
available or in design. Facilities to ion-etch the specimen can also be added.

Fig. 4 Instrument component of the SEM
When the primary electrons interact with the specimen, various signals are generated. A
suitable detector collects and converts one of these to a video signal. The current is then
amplified and used to modulate the intensity or the vertical deflection of the electron beam of
the crt. When the particular property of the specimen changes, the signal strength changes
and, respectively, the brightness or the degree of vertical deflection of the crts beam. The
resulting signal map can be observed on a long-persistence phosphor crt or photographed
from a short-persistence phosphor, high resolution crt.
The great depth of field gives the image a three-dimensional appearance. Because of the
long working distance and the size of the final aperture (140 m variable) the beam
converges on the specimen with a half-angular aperture of a few mili-radians. Thus, at the
object focal plane, the axial extent of the beam which gives a sharp image is relatively large.
The electron beams of the crt and the microscope possess a finite width. To achieve
optimum resolution, the latter should be varied according to a selected magnification, i.e., at a
magnification of 10 x, a l000-line display and a beam diameter of 400 only 0.4% of the
surface is scanned. Hence, the beam size must be increased. The beam width of the crt is
approximately 0.1 mm. Line and frame speed of the 10 cm crt must therefore be adjusted to
1000 lines per frame in order to give a completely covered image. For a continuous visual
display on a long-persistence crt, two frames per set are required. To record an image, frame
times of up to 200 set are necessary. The build-up of a relatively noise-free image within this
time requires a beam current of at least 10
-12
. This means that the beam diameter has to be
larger than 100 ), for conventional tungsten hairpin filaments.
Fig. 5 shows the various mechanisms of signal generation. These signals are generated
when electrons of energies up to 50 kV penetrate the specimen surface and interact with
atoms of the solid. The interaction is known as scattering. The scattering event is a directional
path change of the incident electrons.

Fig. 5 The interactions between the primary electrons () and the host atom
electrons () lead to the generation of a variety of signals
In the Coulomb field of the nucleus the primary electrons are elastically scattered, i.e.,
their path is changed without energy loss.
The majority of scattering events are inelastic collisions with electrons of the host atoms.
The inelastic collision is an energy transfer from the incident electron to the bound electron.
The path of the primary electron is changed and its energy reduced. The bound electron is
excited, or it becomes a free carrier electron, or it leaves the ionized atom. On its path, the
primary electron collides with many electrons until its energy is diminished and insufficient
for further collisions. Depending on their path, a number of scattered electrons escape the
solid. These backscattered electrons become the high energy (>40 eV) region of the
secondary emission. According to the number of scattering events, the high-energy region
consists of singly scattered, plurally and multiply scattered electrons, as it is shown in fig. 6.
The low energy region of the secondary emission reaches a peak at 5-10 eV. This
represents the true secondary electrons. These are ejected from the orbitals of the host atom
by impact ionization. Considering their average diffusion path length and the work function,
the true secondary electrons which can escape the surface are generated within the first 100 A
of the specimen.

Fig. 6 The relative yield of secondary emission as a function of energy
Obviously, the primary electrons and scattered electrons penetrate more than 100 A.
Ejected and excited electrons due to inelastic collisions below the 100 A depth give rise to
additional signals. The time for electrons to remain in a higher energy state is limited. The
return to a low energy state requires the release of part of the electrons energy. This energy
can be lost as heat, or released as a photon or transferred to another electron. The wavelength
of the optical photon is in the UV, visible or IR region of the spectrum. Provided it is not
totally reflected or internally absorbed, it can be collected as a signal. The above mentioned
energy transfer between electrons is one of the many Auger processes. The Auger electron
can be collected, the signal being characteristic for the elements.
If the electron returns from an excited state to an inner orbital, X-radiation is emitted. Its
wavelength is typical for a particular jump within one element. The X-radiation becomes a
characteristic of the elements. On its path through the solid a 10 kV electron could eject some
3000 electrons unless it is backscattered. Usually the total of incident electrons is larger than
the total secondary emission. This means that the absorbed electrons either flow as a current
to ground to maintain electrical neutrality of a conductive specimen or form a charge within
semiconducting or insulating materials. The specimen absorbed current or the beam induced
charge can be collected and utilized as a signal.
All of the above mentioned phenomena are generated by the interaction of primaries and
the solid. The SEM collects one or more of these simultaneously with suitable detectors.
Operating parameters have to be adjusted to optimize each signal. After appropriate
electronic processing a signal map of the specimen is displayed. The display contains typical
information about the area which is scanned by the beam. Depending on which of the signals
is displayed, the SEM is operating in one or another of its various modes (fig. 7).
c. Magnification [1]
Magnification in a SEM can be controlled over a range of up to 6 orders of
magnitudefrom about 10 to 500,000 times. Unlike optical and transmission electron
microscopes, image magnification in the SEM is not a function of the power of the objective
lens. SEMs may have condenser and objective lenses, but their function is to focus the beam
to a spot, and not to image the specimen. Provided the electron gun can generate a beam with
sufficiently small diameter, a SEM could in principle work entirely without condenser or
objective lenses, although it might not be very versatile or achieve very high resolution. In a
SEM, as in scanning probe microscopy, magnification results from the ratio of the
dimensions of the raster on the specimen and the raster on the display device. Assuming that
the display screen has a fixed size, higher magnification results from reducing the size of the
raster on the specimen, and vice versa. Magnification is therefore controlled by the current
supplied to the x, y scanning coils, or the voltage supplied to the x, y deflector plates, and not
by objective lens power.


Fig. 7 The modes and the collectors
d. Resolution of the SEM [1]
The spatial resolution of the SEM depends on the size of the electron spot, which in turn
depends on both the wavelength of the electrons and the electron-optical system that
produces the scanning beam. The resolution is also limited by the size of the interaction
volume, the volume of specimen material that interacts with the electron beam. The spot size
and the interaction volume are both large compared to the distances between atoms, so the
resolution of the SEM is not high enough to image individual atoms, as is possible in the
shorter wavelength (i.e. higher energy)transmission electron microscope (TEM). The SEM
has compensating advantages, though, including the ability to image a comparatively large
area of the specimen; the ability to image bulk materials (not just thin films or foils); and the
variety of analytical modes available for measuring the composition and properties of the
specimen. Depending on the instrument, the resolution can fall somewhere between less than
1 nm and 20 nm. By 2009, the world's highest SEM resolution at high-beam energies (0.4 nm
at 30 kV) is obtained with the Hitachi SU-9000.

4. Sample preparation [1]:
All samples must also be of an appropriate size to fit in the specimen chamber and are
generally mounted rigidly on a specimen holder called a specimen stub. Several models of
SEM can examine any part of a 6-inch (15 cm) semiconductor wafer, and some can tilt an
object of that size to 45.
For conventional imaging in the SEM, specimens must be electrically conductive, at least
at the surface, and electrically grounded to prevent the accumulation of electrostatic charge at
the surface. Metal objects require little special preparation for SEM except for cleaning and
mounting on a specimen stub. Nonconductive specimens tend to charge when scanned by the
electron beam, and especially in secondary electron imaging mode, this causes scanning
faults and other image artifacts. They are therefore usually coated with an ultrathin coating of
electrical conducting material, deposited on the sample either by low-vacuum sputter coating
or by high-vacuum evaporation. Conductive materials in current use for specimen coating
include gold, gold/palladium alloy, platinum, osmium, iridium, tungsten, chromium, and
graphite. Additionally, coating may increase signal/noise ratio for samples of low atomic
number (Z). The improvement arises because secondary electron emission for high-Z
materials is enhanced.
An alternative to coating for some biological samples is to increase the bulk conductivity
of the material by impregnation with osmium using variants of the OTO staining method (O-
osmium, T-thiocarbohydrazide, O-osmium).
Non-conducting specimens may be imaged uncoated using environmental SEM (ESEM)
or low-voltage mode of SEM operation. Environmental SEM instruments place the specimen
in a relatively high-pressure chamber where the working distance is short and the electron
optical column is differentially pumped to keep the vacuum adequately low at the electron
gun. The high-pressure region around the sample in the ESEM neutralizes charge and
provides an amplification of the secondary electron signal. Low-voltage SEM is typically
conducted in an FEG-SEM because the field emission guns (FEG) is capable of producing
high primary electron brightness and small spot size even at low accelerating potentials.
Operating conditions to prevent charging of non-conductive specimens must be adjusted such
that the incoming beam current was equal to sum of out-coming secondary and backscattered
electrons currents. It usually occurs at accelerating voltages of 0.34 kV.
Embedding in a resin with further polishing to a mirror-like finish can be used for both
biological and materials specimens when imaging in backscattered electrons or when doing
quantitative X-ray microanalysis.
The main preparation techniques are not required in the environmental SEM outlined
below, but some biological specimens can benefit from fixation.
5. The application of SEM in surface analysis [5]:
For the majority of SEM studies the secondary mode is used. Surface phenomena and
grain morphologies are studied. The scope of the study is usually to find a relation between
the change in morphology or topography and physical or chemical forces which caused the
change. In other words, the properties of materials are studied or the mechanism of chemical
and physical attacks. Just to mention a few, the respective fields study corrosion, metal
deposition, surface treatment, wear, fractography, plastic deformation, irradiation damage,
and somewhat outside of this schematic, the field of semiconducting materials. A number of
micrographs serve to illuminate the application of the SEM in some of these fields.


Fig. 9 a. CuO wiskers grown on a Cu surface by treatment with a hot oxidizing agent
b. Au-crystallites of an electroless deposited film on a ceramic surface.
c. Needle structure of a Fe
2
O
3
film which has been grown by thermal decomposition of Fe-
carbonyl on a hot stainless steel substrate
d. Topography of a sputtered CdS film
Thin film technology is applied in surface-protective treatment and micro-circuit
fabrication. Deposition conditions obviously determine crystallite size and homogeneity.
These properties alter the performance of the thin films considerably. Figs. 8 show various
thin films. Each micrograph is one example of an entire experimental series in which
numerous deposition conditions have been varied to gain some understanding of the
mechanism of film growth and to find the conditions which reproduce a film of specific
properties.

a
b
c d





Fig. 10 GaP pn-junction with applied 2V
reserved (a); 0V (b); and 8V forward (c) biases






Entire microcircuits and pn-junctions can be observed in the secondary mode. Image
contrast is due to the built-in potential. The potential can be externally varied by applying
biasing voltages. The resulting voltage contrast depends on the trajectories of the escaping
secondary electrons as influenced by the surface fields. Widening and discontinuities of
depletion layer can be observed and attributed to faults in materials or processes. Fig. 10
shows a GaP pn-junction at 0, +2 and -8 V.
6. Summary:
- A scanning electron microscope (SEM) is a type of electron microscope that 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.
- Magnification in a SEM can be controlled over a range of up to 6 orders of
magnitudefrom about 10 to 500,000 times.
- The resolution can fall somewhere between less than 1 nm and 20 nm.
- The useful application of the SEM ranges from surface study to bulk analysis to device
fabrication.
7. References:
[1]. http://en.wikipedia.org/wiki/Scanning_electron_microscope#Beam-
injection_analysis_of_semiconductors
[2]. Bogner et al, A history of scanning electron microscopy developments: Towards wet-
STEM imaging, Micron 38 (2007) 390401
[3]. K D Vernon-Parry, Scanning Electron Microscopy: an introduction, Ill-Vs Review Vol.13
No.4 2000
[4]. C. W. Oatley, The early history of the scanning electron microscope, Journal of Applied
Physics 53, R1 (1982)
[5]. G. W. Kammlott, Some Aspects of Scanning Electron Microscopy, Surface Science 25
(1971) 120-146