Characterization

Complex Engineering Problem

Submitted To:
Muhammad Asif Rafiq
Submitted By:
Isma Rauf (2021-MM-07)

Date:21 December 2023

University of Engineering & Technology, Lahore

Objective:
The objective is the find out the technique to observe the lattice parameters of any material.

Introduction:
A lattice constant or lattice parameter is one of the physical dimensions and angles that
determine the geometry of the unit cells in a crystal lattice, and is proportional to the distance
between atoms in the crystal. A simple cubic crystal has only one lattice constant, the
distance between atoms, but in general lattices in three dimensions have six lattice constants:
the lengths a, b, and c of the three cell edges meeting at a vertex, and the angles α, β,
and γ between those edges.

The length of the unit cell along the x, y, and z direction are defined as a, b, and c.
Alternatively, we can think of the sides of the unit cell in terms of vectors a, b, and c. The
angles between the crystallographic axes are defined by:

α = the angle between b and c

β = the angle between a and c
γ = the angle between a and b

a, b, c, α, β, γ are collectively known as the lattice parameters (often also called ‘unit cell
parameters’, or just ‘cell parameters’).

On this basis there are seven different possible combinations of a, b, and c and 𝛼, 𝛽, and 𝛾,
each of which represents a distinct crystal system. These seven crystal systems are cubic,
tetragonal, hexagonal, orthorhombic, rhombohedral,2 monoclinic, and triclinic. The cubic
system, for which a = b = c and 𝛼 = 𝛽 = 𝛾 = 90°, has the greatest degree of symmetry.

Question 1:
How to measure the lattice parameters?

Answers:
Here are several common methods for measuring lattice parameters:

 X-rays Diffraction
  Neutron Diffraction
 STM
 AFM

Question 2:
Differentiate FCC & BCC structures on the basis of packing density, atom/unit cell and lattice
parameter?

Answer:
Packing Density:

FCC (Face-Centered Cubic): 74%. Closest packing of spheres in layers, with additional
layers in the gaps.

BCC (Body-Centered Cubic): 68%. Less efficient packing due to a lower number of nearest
neighbors.

Atoms per Unit Cell:

FCC: 4 atoms. Atoms at each corner of the cube and one at the center of each face.

BCC: 2 atoms. One at each corner and one at the center of the cube.

Lattice Parameter:

FCC: Smaller lattice parameter compared to BCC for similar elements.

BCC: Larger lattice parameter compared to FCC for similar elements.

Examples:

FCC: Aluminum, Copper, Gold.

BCC: Iron, Chromium, Tungsten.

Question 3:
How the measure lattice parameters when secondary phase come in XRD?

Answer:
1. Make a “stick” plot of I/I1 vs d for the unknown mixture. Perhaps the most useful plot
is I/I1 vs ln d which is easily made on semi-log paper; this allows systematic peak shifts
due to various diffractometer errors to be easily recognized. About 10 or 20 increments
of I/I1 are sufficient.
2. Select likely possibilities (“three strongest lines”, a priori knowledge, hunches) and
make “stick” plots for these knowns based on PDF cards.
 3. Solve the “jig-saw” puzzle, allowing for superposition of lines:
A. Graphically subtract the relative intensities of the first identified phase of the
mixture. Note that the normalization of the identified phase may need to be
changed to match the pattern: the mixture’s most intense peak may not be the
100% peak of the identified phase.
B. Replot the remaining lines (i.e. those with non-zero intensities), renormalizing
the maximum peak to 100% intensity. This is done to allow easy comparison of
the remainder with another phase from the PDF. c. Repeat a. and b. until all
peaks are accounted for.
4. Every line in the pattern must be assigned to some material. All major lines of each
component identified (i.e., of each card) must be present. All remainders from
subtractions must be zero or higher since negative intensities do not exist. In practice,
negative remainders I/I1 less than 0.05 are acceptable. Preferred orientation is often the
cause of less than perfect agreement of intensities

Completing the steps listed above is sufficient for most analyses. For a complete analysis,
however, the following should be done.

5. Prepare mixtures of the identified components until the original diffraction pattern is
duplicated. This step adds considerable reliability to the identification.
6. Compare absolute intensities of the peaks in the unknown and duplicating mixtures to
see if there is any non-crystalline material in the unknown.