CHM 678

PAST YEAR QUESTION

CHAPTER 3
(CRYSTAL STRUCTURE – XRD, SEM TEM)

Name : Wan Nurfatin Nasuha bt Wan Ibrahim (2013682968)

Member : Nur Hafizah bt Adzis (2013876964)
Group : AS2026A1
Lecturer’s name : Tuan Sheikh Ahmad Izaddin Sheikh
Mohd Ghazali
 1. April 2010
A. The first five peaks of a metal powder occur at diffraction angle 2θ= 32.5°, 37.25°,
54.3°, 63.0° and 65.75° when monochromatic x-radiation having a wavelength of
0.00711 nm is used. Given that the lattice constant of the metal is 4.9489 . [Assume
first order diffraction].
Determine:
a) The crystal structure of the metal.(5 marks)

Peaks 2Ɵ Sin2 Ɵ 1x 𝐒𝐢𝐧𝟐 Ɵ 𝐒𝐢𝐧𝟐 Ɵ 𝐒𝐢𝐧𝟐 Ɵ

2x𝐒𝐢𝐧𝟐 Ɵ 3x𝐒𝐢𝐧𝟐 Ɵ h
2 + hkl Ǻ(α)
𝐒𝐢𝐧𝟐 Ɵ 2 2
k +l
1 32.5 0.0783 1.000 2.000 3.000 3 111 0.220
2 37.25 0.1019 1.301 2.603 3.904 4 200 0.223
3 54.3 0.2082 2.659 5.318 7.977 8 220 0.220
4 63.0 0.2730 3.486 6.973 10.46 10 310 0.215
5 65.75 0.2946 3.762 7.525 11.29 11 … 0.217

√(𝝀𝟐 )(𝒉𝟐 +𝒌𝟐 +𝒍𝟐 )

a =
𝟒 𝒔𝒊𝒏𝟐 Ɵ

(𝟎.𝟎𝟕𝟏𝟏𝟐 )(𝟑)
=√
𝟒(𝟎.𝟎𝟕𝟖𝟑)

= 0.220 Ǻ
Confirmation crystal structure =
𝟏.𝟎𝟎𝟎
= 0.77 ~ nearly -0.75 that approve it is FCC crystal structure.
𝟏.𝟑𝟎𝟏

b) The interplanar spacing for the second set of the diffracted planes.(3 marks)
𝛂
dhkl =
√𝒉𝟐 +𝒌𝟐 + 𝒍𝟐

𝟒.𝟗𝟒𝟖𝟗
=
√𝟑𝟐 +𝟒𝟐 + 𝟖𝟐

= 0.5246 Ǻ / 0.05246 nm
 c) Diffraction angel at (331) plane.(3 marks)
𝛂
dhkl =
√𝒉𝟐 +𝒌𝟐 + 𝒍𝟐
𝟒.𝟗𝟒𝟖𝟗
=
√𝟑𝟐 +𝟑𝟐 + 𝟏𝟐

= 1.1354 Ǻ / 0.11354 nm
𝒏𝝀
Sin Ɵ =
𝟐𝒅𝒉𝒌𝒍
(𝟏)(𝟎.𝟎𝟎𝟕𝟏𝟏𝒏𝒎)
=
(𝟐)(𝟎.𝟏𝟏𝟑𝟓𝟒𝒏𝒎)

= 0.0313
Ɵ = 𝒔𝒊𝒏−𝟏 (0.0313)
= 1.794ᵒ
2Ɵ = (2) (1.794ᵒ)
= 3.588ᵒ

B. State the most suitable instrumentation technique in the following characterization

of a titanium alloy:
a) To determine only the surface structure of the alloy.
Scanning Electron Microscope (SEM). Electron source generates electrons
which produced secondary electrons that produce the signal to create the
image. The surface must be electrically conductive by coting it with gold or
platinum.

b) To study the dislocation that occurs in the metal alloy.

Transmission Electron Microscope (TEM). The image seen is formed by an
electron beam that passes through the specimen and then will projected to
a viewable screen for observations and it magnification can approaching
1,000,000x.

c) To determine the concentration of atoms in the titanium alloy.

Optical microscopy where this type of microscopy use light to view and lens
for magnification. Metallographic scopes often use polarized light to
increase contrast (6marks)
2. April 2011
X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission
electron microscope (TEM) are several instruments used in characterization technique
of materials. State a suitable instrumentation technique to be used below:
i) To verify the crystal structure of a metal
X-ray diffraction (XRD)
ii) To observe the presence of dislocation in a crystal structure
Transmission Electron Microscope (TEM)
iii) To study only the surface morphology of a metal
Scanning Electron Microscope (SEM)
iv) To determine the elemental composition in metal alloy
Optical microscopy
v) To determine the interplanar spacing in crystal structure
X-ray diffraction (XRD)
vi) To verify the degree of crystallinity in polymer structure
Optical micsroscopy
(6 marks)

3. January 2012
A. X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission
electron microscope (TEM) are several instruments used in characterizations
techniques of solid materials. Explain sample preparation procedure for each
technique. (6 marks)
(i) XRD – The tungsten filament of cathode is heated, electron are released
by thermionic emission and accelerated through the vacuum by large
voltage and strike the sample. The sample is pressed into a sample
holder so that the samples have a smooth flat surface.

(ii) SEM - the sample will be put on photographic film and the electron will
generates secondary electron to create the signal which use to produce
the image of sample. The surface of sample must be electrically
conductive by coting it with platinum or gold.
 (iii) TEM – the heated tungsten filament will produce electron beam which
passes through very thin foil specimen(3000 – 500 µm) to permit
transmission and bulky material is highly absorptive to electron.

B. An X-ray of Iron (Fe) which is taken using monochromatic x-radiation of

wavelength 0.154 nm shows diffraction peaks at 45.0°, 65.1° and 82.8° which are
identified as (110), (200) and (211) reflection, respectively.
i. Calculate the interplanar spacing and lattice parameter of the peak at
diffraction angle 45.0°. (3 marks)
 = 2dhkl sin θ
 𝟎.𝟏𝟓𝟒
d110 = =
𝟐 𝐬𝐢𝐧 𝜽 𝟐(𝐬𝐢𝐧 𝟐𝟐.𝟓)

= 0.2012 nm
a = dhkl √𝒉𝟐 + 𝒌𝟐 + 𝒍𝟐
a(Fe) = d110 √𝟏𝟐 + 𝟏𝟐 + 𝟎𝟐
a(Fe) = (0.2012)(1.4142)
a(Fe) = 0.2845 nm

ii. Draw all three reflections within a unit cell of Fe.(6 marks)
 iii. Suggest the type of crystal structure for Fe.(3 marks)

Peaks 2Ɵ Sin2 Ɵ 1x 𝐒𝐢𝐧𝟐 Ɵ

𝐒𝐢𝐧𝟐 Ɵ
1 45.0 0.1464 1.0000
2 65.1 0.2895 1.9774
3 82.8 0.4373 2.9870

𝟏.𝟎𝟎𝟎𝟎
= 𝟎. 𝟓𝟎 indicates that it is BCC crystal structure
𝟏.𝟗𝟕𝟕𝟒

C. An unknown material is being analyzed using X-ray diffraction technique.

However, the diffraction patterns are extremely broad (no clear peaks are visible).
What does this tell you about the material? Explain you answer.(3 marks)
We can say that the material is an amorphous materials which do not possess
the periodicity and atom are randomly distributed. X-ray will be scattered in
many direction leading to a large bump and distributed in a wide range instead
of high intensity peaks. On the other hand, crystalline materials are
characterized by the orderly periodic arrangements of atoms and have a sharp
peaks.
4. June 2012
A sample of BCC iron was placed in an x-ray diffractometer using incoming x-rays of
wavelength,=0.1541 nm. Diffraction from the (110) plane was obtained at a
diffraction angle of 44.704°. Calculate a value for the lattice constant (a) of the BCC
iron (assume 1st order diffraction).(4 marks)
2θ=44.704
Θ = 22.352
Sin2θ=0.1446
𝟎.𝟏𝟓𝟒𝟏𝟐
Sin2θ = ( )(12+12+02)
𝟒𝒂𝟐
𝟎.𝟏𝟓𝟒𝟏𝟐
0.1446 = ( )(12+12+02)
𝟒𝒂𝟐
a = 0.1549 nm

5. January 2013
Determine the expected diffraction angle for the first order reflection from the (310) set
of planes for BCC chromium when monochromatic radiation of wavelength 0.0757 nm
is used. Given lattice constant, a = 0.28844 nm. (4 marks)
𝟎.𝟎𝟕𝟓𝟕𝟐
Sin2θ = ( )(32+12+02)
𝟒(𝟎.𝟐𝟖𝟖𝟒𝟒)𝟐

Sin2θ = 0.1722
Sin θ = √𝟎. 𝟏𝟕𝟐𝟐
Sin θ = 0.41497
θ = 𝐬𝐢𝐧−𝟏 𝟎. 𝟒𝟏𝟒𝟗𝟕
θ = 24.52
Diffraction angle, 2θ = 49.04
6. June 2013
If the angle of diffraction for the (321) set of planes occurs at 27 when monochromatic
x-radiation having a wavelength of 0.071nm is used, compute the interplanar spacing
for this set of planes (3 marks)
 = 2dhkl sin θ
 𝟎.𝟎𝟕𝟏
d321 = =
𝟐 𝐬𝐢𝐧 𝜽 𝟐(𝐬𝐢𝐧 𝟐𝟕)

= 0.0782 nm

7. December 2013
A. Determine the expected diffraction angle for the first order reflection from the (110)
set of planes for BCC iron when monochromatic radiation of wavelength 0.1541
nm is used. Given lattice constant, a=0.2865 nm
𝟎.𝟏𝟓𝟒𝟏𝟐
Sin2θ = ( )(12+12+02)
𝟒(𝟎.𝟐𝟖𝟔𝟓)𝟐

Sin2θ = 0.1446
Sin θ = √𝟎. 𝟏𝟒𝟒𝟔
Sin θ = 0.3803
θ = 𝐬𝐢𝐧−𝟏 𝟎. 𝟑𝟖𝟎𝟑
θ = 22.35
Diffraction angle, 2θ = 44.70
 B. X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission
electron microscope (TEM) are several instruments used in characterizations
techniques of solid materials. Explain sample preparation procedure for each
technique.(6 marks)
i) XRD – The tungsten filament of cathode is heated, electron are released
by thermionic emission and accelerated through the vacuum by large
voltage and strike the sample. The sample is pressed into a sample
holder so that the samples have a smooth flat surface.

ii) SEM - the sample will be put on photographic film and the electron will
generates secondary electron to create the signal which use to produce
the image of sample. The surface of sample must be electrically
conductive by coting it with platinum or gold.

iii) TEM – the heated tungsten filament will produce electron beam which
passes through very thin foil specimen(3000 – 500 µm) to permit
transmission and bulky material is highly absorptive to electron.

8. June 2014
Explain briefly the required preparative condition when a titanium alloy structure is to
be examined for the following purposes:
i. To view the surface structure of the alloy by optical micsroscope
Optical microscopy use light to view and lens for magnification where the
titanium alloy must in transparent form. The light source from the top of
titanium alloy flatform for solid sample specimens.

ii. To study the dislocation that occur in the metal alloy by transmission electron
microscope
The titanium alloy must be prepared in very thin foil specimen to permit
transmission of electron beam produced by heated tungsten filament
before projected to a viewable screen for observation because bulky solid
material is highly absorptive to electron beams.
 iii. To examine the surface features of the alloy specimen by scanning electron
microscope
The surface of titanium alloy must be electrically conductive by coting it
with platinum or gold so the electron can generates secondary electron to
produces the signal which use to create the image of sample.

(6 marks)

9. December 2014
A. An X-ray diffractometer recorder chart for an element that has either the BCC or
FCC crystal structure showed diffraction peaks at the following 2θ angles : 41.069,
47.782, 69.879, and 84.396. The wavelength of the incoming radiation was 0.154
nm.
i. Determine the cubic structure of the element (3 marks)
Peaks 2Ɵ Sin2 Ɵ 1x 𝐒𝐢𝐧𝟐 Ɵ 𝐒𝐢𝐧𝟐 Ɵ 𝐒𝐢𝐧𝟐 Ɵ
2x𝐒𝐢𝐧𝟐 Ɵ 3x𝐒𝐢𝐧𝟐 Ɵ h
2 + a(nm)
𝐒𝐢𝐧𝟐 Ɵ 2 2
k +l
1 41.069 0.1230 1.000 2.000 3.000 3 0.3802
2 47.782 0.1640 1.333 2.666 3.999 4 0.3802
3 69.879 0.3280 2.667 5.334 8.001 8 0.3803
4 84.396 0.4512 3.668 7.336 11.00 11 0.3802

𝟏.𝟎𝟎𝟎
=0.75 indicates that this value is for FCC crystal structure
𝟏.𝟑𝟑𝟑

ii. Calculate the lattice constant for the element (3 marks)

Sin2θ=0.1230
𝟎.𝟏𝟓𝟒𝟐
0.1230 = ( )(3)
𝟒𝒂𝟐
a = 0.3802 nm
𝟎.𝟑𝟖𝟎𝟐+𝟎.𝟑𝟖𝟎𝟐+𝟎.𝟑𝟖𝟎𝟑+𝟎.𝟑𝟖𝟎𝟐
average lattice constant,a = = 0.3802 nm
𝟒
B. X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission
electron microscope (TEM) are several instruments used in characterizations
techniques of solid materials. Explain sample preparation procedure for each
technique.(6 marks)
i) XRD – The tungsten filament of cathode is heated, electron are released
by thermionic emission and accelerated through the vacuum by large
voltage and strike the sample. The sample is pressed into a sample
holder so that the samples have a smooth flat surface.

ii) SEM - the sample will be put on photographic film and the electron will
generates secondary electron to create the signal which use to produce
the image of sample. The surface of sample must be electrically
conductive by coting it with platinum or gold.

iii) TEM – the heated tungsten filament will produce electron beam which
passes through very thin foil specimen(3000 – 500 µm) to permit
transmission and bulky material is highly absorptive to electron.
10. June 2015
The diffraction pattern for polycrystalline α-iron is shown below:

i) calculate the interplanar spacing and lattice parameter for each of the peaks (6
marks)
2θ=45
 = 2dhkl sin θ
 𝟎.𝟏𝟓𝟒
d110 = =
𝟐 𝐬𝐢𝐧 𝜽 𝟐(𝐬𝐢𝐧 𝟐𝟐.𝟓 )

= 0.2012 nm
a = dhkl √𝒉𝟐 + 𝒌𝟐 + 𝒍𝟐
a(Fe) = d110 √𝟏𝟐 + 𝟏𝟐 + 𝟎𝟐
a(Fe) = (0.2012)(1.4142)
a(Fe) = 0.2845 nm

2θ=65.1
 = 2dhkl sin θ
 𝟎.𝟏𝟓𝟒
d200 = =
𝟐 𝐬𝐢𝐧 𝜽 𝟐(𝐬𝐢𝐧𝟑𝟐.𝟓𝟓 )

= 0.1431 nm
a = dhkl √𝒉𝟐 + 𝒌𝟐 + 𝒍𝟐
a(Fe) = d200 √𝟐𝟐 + 𝟎𝟐 + 𝟎𝟐
a(Fe) = (0.1431)(2)
a(Fe) = 0.2862 nm
 2θ=82.8
 = 2dhkl sin θ
 𝟎.𝟏𝟓𝟒
D211 = =
𝟐 𝐬𝐢𝐧 𝜽 𝟐(𝐬𝐢𝐧 𝟒𝟏.𝟒)

= 0.1164 nm
a = dhkl √𝒉𝟐 + 𝒌𝟐 + 𝒍𝟐
a(Fe) = d211 √𝟐𝟐 + 𝟏𝟐 + 𝟏𝟐
a(Fe) = (0.1164)(2.4495)
a(Fe) = 0.2852 nm

ii) From the diffraction peaks, suggest the type of crystal structure for α-Fe(2 marks)

Peaks 2Ɵ Sin2 Ɵ 1x 𝐒𝐢𝐧𝟐 Ɵ

𝐒𝐢𝐧𝟐 Ɵ
1 45.0 0.1464 1.0000
2 65.1 0.2895 1.9774
3 82.8 0.4373 2.9870

𝟏.𝟎𝟎𝟎𝟎
= 𝟎. 𝟓𝟎 indicates that it is BCC crystal structure
𝟏.𝟗𝟕𝟕𝟒

iii) Illustrate each reflection (110), (200) and (211) within a unit cell of the metal
( 6 marks)