Name: ______________________

Student Number: _____________

MECH 4430 – Materials Characterization

Assignment 2 on March 11th, 2020 – Due date March 25th, 2020

Answer all questions (100 points in total)

1. Multiple choice questions (4 marks X 10 questions = 40 marks)

(Please indicate the most correct answer, no partial marks will be given.

Question 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.9 1.10
Answer D B D D C D D D A D

1.1 The optical path of a transmission

electron microscope (TEM) is shown
in the figure on the right. TEM can
switch between image mode (b) and
diffraction mode (a). According to
the figure shown, which of the
following is responsible to switch
between image mode and
diffraction mode?
(A) Objective lens
(B) Objective aperture
(C) SAD (selected area aperture)
(D) Intermediate lens

1.2 Which of the following is the source that generates the contrast in TEM images?
(A) Different capability of absorption of electrons by specimen
(B) Different number of electrons that scattered or diffracted by different part of specimen
(C) X-rays that emitted during TEM process
(D) None of the above

1.3 Mass-density contrast and diffraction contrast are the main mechanism of contrast in TEM. Which
of the following is incorrect about the contrast generated in various specimens?
(A) Mass density contrast is generated in polymeric and biological specimens (mainly amorphous)
(B) Diffraction contrast is generated in crystalline specimens
(C) Polymeric and biological specimens are often stained with heavy-metal oxides to increase the
mass density contrast
(D) Mass density contrast is generated in polymeric and biological specimens ONLY

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 Name: ______________________

Student Number: _____________

1.4 Which of the following is/are possible observations using diffraction mode in TEM?
(A) Bright field images
(B) Dark field images
(C) Diffraction patterns by selected -area diffraction
(D) All of the above

1.5 Kikuchi lines are pairs of parallel lines consisting of one bright and one dark line in the diffraction
mode. Which of the following statement is NOT true about formation of Kikuchi lines?

(A) Kikuchi lines are formed due to inelastic scattering of electrons in a specimen

(B) A cone of electron rays to all direction is formed by the primary incident rays of electrons

(C) The bright and dark lines are not formed by the electron rays that satisfy Bragg conditions.

(D) Kikuchi lines are used to guide the specimen tilting

1.6 Both TEM and SEM use the signal sources (electrons) during electron interaction with specimen.
Which of the following is NOT true about the difference of imaging principles between TEM and SEM?

(A) TEM uses either the transmitted electrons or the diffracted electrons to form images
(B) SEM uses either the secondary electrons (SEs) or backscattered electrons (BSEs) to form images
(C) The specimen for SEM analysis could be in various form, i.e. bulk (relatively thick), or powder, or
thin film.
(D) No special requirement is needed to TEM’s sample preparation

1.7 In SEM, both secondary electrons (SEs) and backscattered electrons (BSEs) are used as useful signals.
_ (!)_ scattering produces BSEs, which are incident electrons scattered by atoms in the specimen. _ (2)_
scattering produces SEs, which are electrons ejected from atoms in the specimen (often on surface).
BSEs are typically deflected from the specimen at large angles and with _(3)_ energy loss. The number of
BSEs from a specimen depends on the _(4)_ number. On the contrary, SEs are typically deflected at
small angles and show much _(5)_ energy compared with incident electrons. Which of the following
shows the correct contents for (1) – (5)?

(A) (1) Inelastic; (2) Elastic; (3) high; (4) atomic; (5) higher
(B) (1) Elastic; (2) Inelastic; (3) high; (4) outermost shell electron; (5) lower
(C) (1) Inelastic; (2) Elastic; (3) little; (4) atomic; (5) lower
(D) (1) Elastic; (2) Inelastic; (3) little; (4) atomic; (5) lower

1.8 Both topographic and compositional contrast are used in SEM imaging. Which of the following
statement is true about the contrast formation of SEM images?

(A) Topographic contrast results from the variation in geometric features on the specimen surface
(B) Compositional contrast arises due to the variation in chemical composition in a specimen, i.e.
capability of BSEs escaping from the specimen depends on the atomic number of the specimen.
(C) For a specimen made of a uniform material (same element) with a rough surface, we should use
the SEs to form a SEM image.

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 Name: ______________________

Student Number: _____________

(D) All of above

1.9 The resolution of SEM imaging is determined by the cross-sectional diameter of the scanning probe.
Which of the following statement is NOT true?

(A) Probe current should be reduced in order to minimize the probe diameter
(B) Higher voltage should be applied in order to increase the brightness
(C) Higher voltage should be applied in order to reduce the electron wavelength
(D) A threshold probe current should be maintained in order to have object contrast in SEM

1.10 In order to achieve the 3-D appearance of topographic SEM images, we need to maintain a
2𝑅
reasonable depth of field 𝐷𝑓 = . Which of the following control(s) depth of field?
𝑡𝑎𝑛𝛼

(A) Working distance

(B) Aperture diameter
(C) Convergence angle of electron beam
(D) All of the above

2 (Total 10 marks)
(1) What is the special requirement for TEM’s specimen preparation. (4 marks)

The specimen has be machined and prepared thin enough to allow electrons pass through it.

(2) Briefly describe the sample preparation method of metal, ceramics and polymer for TEM
inspection.. (6 marks)
• Electropolishing for metal specimens, where the surface materials are dissolved in a
electrolytic cell containing acidic solutions and specimens thickness is reduced (2
marks)
• Ion milling for both metal and ceramic specimens, where energetic ions bombard on
the specimen surface and knock away the surface materials (2 marks)
• Ultra-microtomy for polymer and biological specimens, where the material is
removed by glass or diamond knife (2 marks)

3 Please include necessary angles and Miller index of spots when sketching the following. (Total 20
marks)
(1) Please sketch diffraction pattern of face-centered cubic (FCC) single crystal with transmitted
beam direction B=[001]. (10 marks) Please show the process how you have arrived in indices for
each spot in the diffraction pattern.
Answers:

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 Name: ______________________

Student Number: _____________

Before sketching the diffraction spots in reciprocal space, we shall bear in mind the structural
extinction rules (in Chapter 2 – XRD). Crystallographic planes that can be identified in diffraction
method:
FCC: 111, 200, 220, 311, 222, 400, 331, 420, …

And other reciprocal vectors ( such as

R(400) , R(420) , etc.) can also be obtained by
further translation of R(200) , R(020) , and
R(220) by various lengths. And finally the
figure on the right is obtained.

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 Name: ______________________

Student Number: _____________

(2) Please sketch diffraction pattern of body-centered cubic (BCC) single crystal with transmitted
beam direction B=[001]. (10 marks) Please also show the process how you have arrived in
indices for each spot in the diffraction pattern.
Crystallographic planes that can be identified in diffraction for BCC is the planes of 110, 200, 211,
220, 310, 222, 321, 400, …

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 Name: ______________________

Student Number: _____________

And other reciprocal vectors can also be

obtained by further translation of R(200) ,
R(020) , R(220) and R(110) by various lengths.
And finally the figure on the right is
obtained.

4 Compare light microscopy (5 marks), transmission electron microscopy (TEM) (5 marks), and
scanning electron microscopy (SEM) (5 marks) in terms of illumination source, imaging formation
mechanism, and specimen preparation. (You are suggested to tabulate these items for comparison
of the three characterization methods.) (Total 15 marks)

Comparison Light microscopy Transmission electron Scanning electron microscopy

microscopy (TEM) (SEM)

Illumination source Visible light High energy electrons High energy electrons

Image formation Visible light is focused High energy electrons are High energy electrons are focused
mechanism by glass lens and form focused by by electromagnetic lens and
images of specimen electromagnetic lens and scanned across the specimen
surface. Image contrast the transmitted electron surface. Images are formed by
is due to difference in beam form images of either the backscattered electrons
reflecting or absorbing specimen surface. The (BSE, incident electron beam
visible light by different image contrast results elastically scattered) or by
areas of surface. from the difference in the secondary electrons (SE, electron
number of electrons that emitted from specimen by
are scattered away from inelastically scattering). The image
the transmitted beam, i.e. contrast results from topographic
mass-density contrast and contrast (e.g. BSEs) or
diffraction contrast. compositional contrast (e.g. SEs).

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 Name: ______________________

Student Number: _____________

Specimen Usual procedures Specially, the specimen Usual procedures involve cutting
preparation include cutting, needs to be reduced in and cleaning to remove surface
mounting (moulding), thickness so that electrons contaminants. For electrically non-
grinding / polishing, and can transmit through it. conductive specimens, conductive
etching coating needs to be applied by
sputtering.

5 (Total 15 marks)
(1) The figure below is an SEM image with compositional contrast formed by backscattered
electrons (BSE). According to the contrast shown in area A (grey) and B (black), which area
contains elements with relatively higher atomic numbers ? Please explain (8 marks)

Answer: Since area A appears brighter than area B,

therefore, area A contains elements with relatively
higher atomic number. Because backscatter
coefficient increases monotonically with the
increase of atomic umbers, i.e,, elements with higher
atomic number will generate more number of
backscattered electrons, which are captured by the
detector of SEM, thus, the area appears brighter in
the SEM image.

(2) The figure below is an SEM image with topographic contrast formed by secondary electrons (SE).
According to the contrast shown in surface C (bright) and surface D (dark), what information
can we get from this contrast? Please explain (7 marks)

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 Name: ______________________

Student Number: _____________

Answer:

Since surface C appears brighter than surface D,

therefore, surface C is more favorably facing the
detector, so the detector receives more electrons
from surface C than from surface D.