Topographic Contrast

 Topographic contrast in an SEM refers to variation in signal levels that corresponds

to variation in geometric features on the specimen surface.

Topographic contrast occurs because signal electrons arise from two effects:
-the trajectory effect and
-the electron number effect

 The electrons emitted from the specimen surfaces facing the detector will be collected
abundantly, and corresponding sites in the image will appear bright.

 The electrons emitted from the surfaces not facing the detector will reach the detector with
difficulty, and thus corresponding sites in the image will appear dark.
 The electron number effect will create bright areas in the image that do not correspond to
surface contours on the specimen.

 When the electron probe hits near an edge or a inclined surface, more electrons can
escape from the specimen than when the probe hits a flat surface directly. Thus,
certain areas of the specimen (such as edges of spherical particles, raised areas, and cavities)
will appear bright in an SEM image
Compositional Contrast
 Compositional contrast refers to the variation in gray levels in an SEM image that
correspond to variation in chemical composition in a specimen.
 The origin of compositional contrast arises because the capability of BSEs to escape from
the specimen depends on the atomic numbers of the specimen atoms.
 The backscatter coefficient (η) characterizes such capability

 η is the ratio of the number of BSEs escaping from the specimen (nBSE) to the number of
incident electrons (ni) and increases monotonically with the atomic number
 Any area in a specimen containing chemical elements
with higher atomic number will generate more BSEs.

 The difference in the number of BSEs collected by a

detector will appear as differences in gray levels
in a black and white image that is, an area with atoms of
higher atomic numbers will appear brighter. Thus, a
BSE image shows the atomic number contrast or
compositional contrast
 SE BSE
 When the E–T detector is used for compositional contrast, the Faraday cage should be
negatively charged (−50 V) to exclude SEs with energies lower than the bias voltage of the
cage.

 Some SEM systems are equipped with a dedicated detector for BSE collection, which is
placed above the specimen. To obtain compositional contrast, we can switch detection from
the SE mode to the BSE mode by simply pushing a button on the SEM control panel.
Operational Variables

 A good SEM image can be obtained by adjusting desired depth of field and resolution.

 How you will control the depth of field and resolution?

-by adjusting operation variables such as the working distance, final aperture size,
acceleration voltage, probe current, and astigmatism.

Working Distance and Aperture Size

The working distance and aperture size are the operational variables that strongly affect
depth of field.

The depth of field is related to the

resolution (R) and the convergence
angle of objective aperture (α)

The resolution of an SEM image on a display screen is limited by the pixel size of the
screen.
the pixel size = resolution X the SEM magnification (M)
αf is controlled by the final aperture radius and the working distance between the aperture
and specimen surface .

Above equation can be rewritten to express the depth of field as a function of the aperture
radius (Rfap) and the working distance (DW) as follows.
 A small aperture size and a long working distance
results in a high depth of field.

 Although selecting a combination of small

aperture size and long working distance is
favorable for high depth of field, such operation
will result in negative effects on image resolution.

 A small aperture size reduces the probe current, and also may reduce the ratio of signal-to-
noise.
 A long working distance is not desirable because it will decrease αf if the aperture size is
unchanged. A small αf is not favorable for high resolution.
 A long working distance increases the spherical aberration of a lens and consequently worsens
the SEM resolution.

 Considering such trade offs between resolution and depth of field, it is wise to select an
intermediate aperture size and intermediate working distance, unless a very large depth
of field or very high resolution is required.
Acceleration Voltage and Probe Current
 The probe size and probe current are critical to achieving high-resolution SEM images.

 The acceleration voltage of the electron gun, and probe current, are two primary operational
variables used to adjust the resolution.
 Increasing the acceleration voltage, which is equivalent to decreasing the wavelength, will
reduce the probe size. The benefit of voltage increase is reflected in increases in electron
beam brightness, which also results in reduction of the probe size.

 The negative effects of selecting higher voltage, which are due to the interaction between
electron probe and specimen materials, should not be ignored.
 In a field-emission SEM system, a relatively low acceleration voltage (∼5 kV) can also
achieve high electron beam brightness and a small probe size.
Astigmatism
 Astigmatism is an operational variable that is often adjusted to obtain a good electron
microscope image. Astigmatism is the lens aberration resulting from power differences of a
lens in its lens plane perpendicular.

 For most SEM systems, astigmatism is not a serious problem when magnification of the
image is less than 10,000×. At high magnification, astigmatism effects on an image are seen.
An image with astigmatism looks out of focus.

 This can be conveniently corrected using the stigmator knobs on the SEM control
panel. The stigmator adjusts the electromagnetic field of the objective lens in two
perpendicular directions in order to eliminate the asymmetrical distortion of the lens.
Specimen Preparation
 A specimen for SEM analysis can be in any form; such as bulk, powder, thin film, and so on.
This is one of reasons that SEMs are more widely used than TEMs.

 There are special problems in SEM specimen preparation such as surface charging of
specimens that have poor electric conductivity, and dehydration requirement for
biological samples.

Preparation for Topographic Examination

 The preparation should involve only sizing the specimens to fit a SEM specimen holder and
removing surface contaminants.
 Common contaminants on the specimen surfaces are hydrocarbons from oil and grease,
because an electron beam decomposes any hydrocarbon and leaves a deposit of carbon on
the surface.
Charging and Its Prevention
 Surface charging is most likely encountered when examining electrically nonconductive
surfaces.

 Charging causes image distortion and artifacts because the charged regions deflect the
incident electron probe in an irregular manner during scanning

 Surface charging should be a primary concern for nonconductive specimens such

as ceramics, polymers, and specimens containing biological substances.

 Surface charging is generally not a problem for metallic specimens because their good
electrical conduction ensures removal of excess electrons
 Prevention
 The most common way to prevent charging is to coat a conductive film onto specimen
surfaces to be examined. Conductive coating is ordinarily accomplished by means of either
vacuum evaporating or sputtering. Vacuum evaporating deposits conductive atoms on a
specimen in a vacuum chamber.

 Vacuum evaporating deposits conductive atoms on a

specimen in a vacuum chamber. The conductive
substance has to be heated to a high temperature for it to
evaporate.

 Sputtering strikes a conductive target with high-energy

ions that impart momentum to atoms of the target,
enabling them to leave the target and deposit on the
specimen.

 The coating thickness is normally controlled at about 5–20 nm depending on the

magnification to be used in SEM examination. High-magnification imaging requires a thin
coating, 5 nm or less.
 Heating of the specimen during coating can cause cracking, pitting, and melting,
particularly for organic specimens. To avoid these problems, cool sputtering, known as
plasma–magnetron sputtering, can be used.
Preparation for Microcomposition Examination

Any specimen prepared for topographic examination is generally suitable for

composition examination using the BSE mode. Electrical conduction of specimen
surfaces is still required for compositional examination.

A specimen prepared for light-microscopy examination may also be directly used for
composition examination in an SEM. If the specimen is either not metallic or is a metallic
specimen mounted in a nonconductive substrate, we should coat the specimen for composition
examination as for topographic examination.

The etching used for light microscopy is not necessary for compositional contrast using the
BSE mode, while deeper etching is required for topographic contrast using the SE mode.

For polymer specimens, we can use a heavy-metal element to stain the specimens to generate
compositional contrast, similar to preparing polymer specimens
for TEM. Compositional contrast resulting from staining can reveal a polymer
specimen containing multiple phases because the staining level of the heavy-metal
element varies with molecular structures of polymer phases.

Dehydration
 ST 3
Marks 10
Time allowed 10 Minutes

1. What type of element indicates from bright phase of a SEM BSEs

image ? 2
2. What type of contrasts are obtained from SEs and BSEs? 2
3. What is the effect of astigmatism on SEM image? 2
4. Why does the following SEM image shows the bright line and dark
area? 4