Name NURZAWANAH AKMAR BINTI

HASBULLAH
(2017840202)
Course Code MST613

Group AS2305M1

Title of Experiment EXPERIMENT 2 : MICROSTRUCTURE

OBSERVATION BY SCANNING ELECTRON
MICROSCOPY, SEM

Lecturer’s Name DR MOHD MUZAMIR MAHAT

Partner’s Name NURSAHIRA BINTI CHE MAT (2017428078)

MUHAMMAD IMAN ILYAS BIN RAZALI
(2017863566)
NIK NORSAMIHAH BINTI AZIZ
(2017489754)
DANIA ADILA BINTI AHMAD RUZAIDI
(2017459498)
NURAMIRAH HASNI BINTI MOHAMAD
HIZAM (2017845864)
NUUR FARRAH SYAHIRAH BINTI
MUHAMAD DUZUHRI (2017421896)
FATIN AMIRA BINTI ABDUL MALEK
(2017879658)
NURAFIQAH BINTI MOHD FAUDZI
(2017486498)

Date 8 OCTOBER 2019

OBJECTIVES

a)   To track the SEM spectroscopy process.

b)   To study the details of the mechanism in SEM spectrocopy.

INTRODUCTION

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.

Source of electrons

In standard electron microscopes electrons are mostly generated by heating a tungsten filament by
means of a current to a temperature of about 2800°C. Sometimes electrons are produced by a crystal of
lantanumhexaboride (LaB6) that is mounted on a tungsten filament. This modification results in a
higher electron density in the beam and a better resolution than with the conventional device. In a field
emission (FE) scanning electron microscope no heating but a so-called "cold" source is employed. An
extremely thin and sharp tungsten needle (tip diameter 10–7 –10-8 m) functions as a cathode in front
of a primary and secondary anode. The voltage between cathode and anode is in the order of magnitude
of 0.5 to 30 KV. Because the electron beam produced by the FE source is about 1000 times smaller
than in a standard microscope, the image quality is markedly better. As field emission necessitates an
extreme vacuum (10-8 Torr) in the column of the microscope, a device is present that regularly
decontaminates the electron source by a current flash. In contrast to a conventional tungsten filament,
a FE tip last theoretically for a lifetime, provided the vacuum is maintained stable.

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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 "activators"
(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. Backscattered
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.

MATERIALS

Polyaniline fiber sample

Fe3O4 sample

APPARATUS

SEM machine
Sample holder

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METHOD

1.   The sample was grind, polished and etched to get a smooth surface before run into the SEM. 

2.   The chamber was opened and the sample was put on the sample holder. 

3.   The chamber was closed by sliding it shut once the sample is in place. Wait about 15 minutes to
vent out the vacuum. 

4.   The User Tool Bar was clicked to select the secondary electron detector. 

5.   The X-Y Zeiss Joystick was clicked to select and identify the features of interest for image capture
and the fine focus adjustment was started.
6.   The stigmator X and Y was used to tune the image by go back and forth beyond the stigmatism
point so that clearly image was seen. 

7.   Once desired focus is achieved, the image was captured by selecting the scanning option at the
SEM control panel. 

8.   The image was saved at TIFF file. 

9.   The Backscattered Detector (BSD) and In Lens detector was continued to see the different images.



PRECAUTIONS

1. Do not open the chamber while the alarm red light is on.
2. Never touch the detector (may result in signal off).

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DATA/RESULTS

1. Polyaniline fiber sample

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SEM and EDS analysis results of PS (500x magnification)

Mapping analysis to show the present of C, O and N

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 Purple spot represent C-K,

Yellow spot represent O-K and Red spot represent N-K.

Total Carbon, Oxygen and Nitrogen present at the spot

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2. Fe3O4 sample

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 Total Oxygen and Iron present in the spot

Red spot present O-K and green present Fe-KA

Mapping analysis to show the present of Fe and O

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 Total Oxygen and Iron present in the spot

SEM and EDS analysis of Fe3O4 (500x magnification)

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DISCUSSION

Throughout this experiment, we managed to learn how SEM works. The main SEM
components include:

§   Source of electrons
§   Column down which electrons travel with electromagnetic lenses
§   Electron detector
§   Sample chamber
§   Computer and display to view the images

Electrons are produced at the top of the column, accelerated down and passed through a combination
of lenses and apertures to produce a focused beam of electrons which hits the surface of the sample.
The sample is mounted on a stage in the chamber area and, unless the microscope is designed to operate
at low vacuums, both the column and the chamber are evacuated by a combination of pumps. The level
of the vacuum will depend on the design of the microscope.

The position of the electron beam on the sample is controlled by scan coils situated above the objective
lens. These coils allow the beam to be scanned over the surface of the sample. This beam scanning, as
the name of the microscope suggests, enables information about a defined area on the sample to be
collected. As a result of the electron-sample interaction, a number of signals are produced. These signals
are then detected by appropriate detectors.

For the first sample which is polyaniline fiber sample is a non-conductive material and therefore does
not have enough supply of electron. The specimen is lined with gold before the SEM analyses the
polyaniline sample. Figure 4 shows the SEM and EDS findings for the polyaniline surface layer. SEM
analytical results show different patterns of particle size. The particle patterns at magnification 500x
can clearly be seen in Figure 6. Nanotubes like the structure are shown in the results. The findings of
the EDS review show the sample composition C, O and N. Graph 2 shows the O level above Fe, and
the mapping analysis shows that the amount of nitrogen relative to oxygen and carbon is smaller. The
sum of each element contained in the sample from Table 3 can be seen as support for analysis. Because
polyaniline is a non-conductive specimen, the supply of electron is inadequate, therefore we can see
charge in the image.

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Next we have the Fe3O4 sample, SEM and EDS tests of the ferrous ferric oxide derived surface layer
Fe3O4 will be shown. There are a variety of specific size variations in the outcome of the study using
SEM. Figure 1 shows that for each magnification the particle appears to be approximately circular. The
output in the form of the composition and morphology of the material is provided when a sample is
tested via SEM. The findings of EDS analyzes show the composition in the Fe and Oxygen, O test. The
O level is greater than Fe from Graph 1 and more oxygen than Fe is seen in the mapping analysis. The
sum of element Fe and O in the test of Table 1 is shown to help the analysis. A number of elements Fe
and O are present at certain levels, such as Tables 1 and Table 2. For example. Because Fe3O4 is a
conducting sample, there is enough electron supply for the image to be viewed.

The main reason for coating or reducing the bulk conductivity of a non-conductive sample is to improve
the electric conductivity of the sample. Highly resistive materials, i.e. more than 1010 Q m, easily load
under the incident beam and can establish a potential that is adequate for a dielectric breakdown in
sample regions. This results in surface potential changes, leading to complex and dynamic picture
artifacts known as' loading.' The artefacts display deflecting secondary low-energy electrons, the
secondarily emissions from raw samples, frequent blasts of secondary electron emissions, and electron
beam deflection, which all weaken the system's solving and analysis power by producing astigmatism,
instabilities, undue luminosity and spurious ray-x This undesirable condition is often made harder
because many of the adhesion materials used to bind the samples to the substratum are non-conducting
and do not leak free from any electrical charge, even conductive specimens. Silver or carbon paint may
set an acceptable conduction path but if only electric conductance is involved, a thin layer of coating,
gold, silver or copper will be sufficient to avoid charging problems. Although metallic specimens will
normally be conducting, often non-conductive areas, such as inclusions, may want to be investigated
and in such cases a thin layer must be applied. To order to ensure that samples current is drained onto
the ground without a large surface potential, the conductivity of the thin film should be enough.

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QUESTIONS

1.   Give 3 possible source of signal with the SEM. Differentiate between elastic and inelastic
scattering. 


Possible source of signal with the SEM :

- Secondary electrons
- Backscattered electrons
- X - Rays

Elastic scattering occurs when there is no loss of energy of the incident primary electron. Elastically
scattered electrons can change direction but do not change their wavelength. Coherent elastic scattering
produces the effect of electron diffraction, which is used to analyze crystal structure.

Inelastic scattering occurs when there is an interaction that causes loss of energy of the incident primary
electron. Inelastically scattered electrons have a longer wavelength. Inelastic scattering occurs by many
mechanisms, and the energy is transferred to the specimen generating a range of useful signals that are
exploited to characterize the material.

2.   Name the detector available for FESEM, Carl Zeiss. 


Everthart-Thorniey, solid state detector and energy dispersive spectrometer (EDS).

3.   Why non-conductive sample need to be coated? Does the thickness of coating would affect the
analysis? Why? 


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 electrically 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.

Thin layer is typically considered to be between 5-50nm -not thick enough to mask surface morphology
but enough to provide a conductive coating to dissipate charging artifacts, any resultant heat buildup
and minimize beam damage.

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CONCLUSION

In conclusion, we had successfully observed the process in SEM spectroscopy where the specimen that
we used are polyaniline fiber and Fe3O4 sample. Both sample shows different properties and elements
depending on its microstructure. Next, we also managed to learn more details about the mechanism in
SEM spectroscopy. The SEM focuses an electron beam at a point on the surface of the sample and then
measures the resulting electrons with a detector. By doing this in a raster pattern across the surface an
image is formed, pixel by pixel. At the top of the image is the column where the electron beam is
generated and focused. From the column comes the electron beam, also called the primary electrons,
shown here in blue. When the primary electrons impact the surface they generate secondary electrons,
backscattered electrons, Auger electrons, X-ray photons and cathodeluminescence.

REFERENCES

1. B.J. Inkson, in Materials Characterization Using Nondestructive Evaluation (NDE) Methods (2016).
Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) for materials
characterization. Retrieved from https://www.sciencedirect.com/topics/chemistry/elastic-scattering

2. Science Education Resource Centre (2017). Scanning Electron Microscopy (SEM). Retrieved from
https://serc.carleton.edu/research_education/geochemsheets/techniques/SEM.html

3. Hayley Anderson (2010). Advantages and Disadvantages in Imaging Components and

Applications. Retrieved from https://www.microscopemaster.com/scanning-electron-microscope.html

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ATTACHMENTS

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