S C A N N I N G E L E C T R O N

M I C R O S C O P Y
A N D
E N E R G Y D I S P E R S I V E
X - R A Y S P E C T R O S C O P Y

PH 762 EXPERIMENTAL
TECHNIQUES
DR. ZULQURNAIN ALI
 Scanning Electron Microscope

• The SEM uses a beam of high energy electrons generated by an

electron gun, processed by magnetic lenses, focused at the specimen
surface and systematically scanned across the surface of a specimen.
• A series of electromagnetic lenses and apertures are used to reduce
the diameter of the electron source and to place a small, focused
beam of electrons onto the specimen.
• High vacuum mode is the normal mode of operation for the SEM. A
high vacuum minimises scattering of the electron beam before it
reaches the specimen.
• The specimen holder is fixed to the specimen stage. The stage can be
moved manually along the X, Y (in the specimen plane), and Z
directions (at right angles to the specimen plane). The Z adjustment is
also known as the specimen height. Most specimen stages will also
rotate and tilt the specimen.
 Scanning Electron Microscope

Once the electron beam reaches and interacts with the sample there are several different kinds of signal that
can be detected. The most commonly used signals are secondary electrons, backscattered electrons and X-Rays
Secondary electron imaging (SEI) is ideal for recording topographical information. A common type of SE detector is the
Everhart-Thornley detector.

The backscattered electron detector (BSD) is mounted

below the objective lens pole piece and centred around
the optic axis. BSE have higher energies than secondary
electrons and can give us information from below the
surface of the sample.

The most common system for detecting the X-rays emitted from the sample
is the energy dispersive X-ray spectrometry (EDS). The EDS detector is
based on a semiconductor crystal. The two most common types are the
lithium-drifted silicon (SiLi) and the silicon drift detector (SDD).
Secondaray Electrons, Back scatter Electrons and X-Rays
 SEM Image

Contrast
It is a measure of the real information in the signal and related to the properties of
the specimen (shape, composition, etc.) that we wish to determine.
Compositional (Atomic Number) contrast
It arises because the intensity of the signal generated from areas with different
composition is proportional to the difference in the average atomic number of the
respective areas.
Topographic contrast
It includes all effects by which the shape and morphology of the specimen can be
imaged.
 Sample Prepration for SEM analysis

To increase the yield of SE emitted from the specimen, heavy metals such as gold or platinum are routinely
used to coat specimens. An extremely thin layer is applied (~10 nm). This coating is applied for two main
reasons:
1. Non-conductive specimens are often coated to reduce surface charging that can block the path of SE and
cause distortion of signal level and image form.
2. Low atomic number (Z) specimens (e.g. biological samples) are coated to provide a surface layer that
produces a higher SE yield than the specimen material.
Once the sample is fully dried it can be mounted on an SEM stub and then coated with a thin layer of a
conductive. If the sample is inherently conductive it will not require coating.
Energy-Dispersive X-ray Analysis (EDX or EDS)

Influence of annealing on microstructure and optical

properties of hot wall deposited PbxSn(1 − x)S thin films

Thin Solid Films 616 (2016) 773–779