Université Française d'Égypte

Prépa 2
PRE 210 Materials Properties
TP
2023-2024

Lab Report 1

Microstructure analysis of metals.

Name: Habiba Islam, Yassin Elwakil

Dr. Rania ElAnwar

ABSTRACT
 This report discusses the analysis of metal’s structure on a microscopic scale
using x-ray diffraction. There are various ways to analyze the microstructure of the
material depending on the requirements of the analysis. These include the desired
level of detail, resolution, sample size, and the need for surface or internal
information. Seeing where it all started with the work of Max Von Laue and the
Bragg’s in the early 20th century and since XRD has evolved into a trusted
instrument for showing the details of crystalline structures. The manufacturing
process has 6 key components as the X-ray tube, crystal monochromator, sample
stage, and detector to find in the end detailed diffraction patterns. Of course, XRD
provides great advantages in the identification phase, quantitative analysis, and
crystallographic insights. But it still has limitations such as surface sensitivity and
the need for crucial sample preparation. Understanding the principles and the
process of the XRD shows its extremely important role in increasing our
knowledge about microstructure in metals.

TABLE OF CONTENT

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S
ABSTRACT..........................................................................................................................

TABLE OF FIGURES:.........................................................................................................

INTRODUCTION................................................................................................................

HISTORY BEHIND X-RAY DIFFRACTION:....................................................................

OBJECTIVES.......................................................................................................................

HOW XRD WORKS AND ITS PROCESS:........................................................................

PHYSICAL VIEW:...............................................................................................................

ADVANTAGES AND DISADVANTAGES:........................................................................

CONCLUSION:....................................................................................................................

REFERENCES:..................................................................................................................

TABLE OF FIGURES:
Fig(1) x-ray diffraction camera.............................................................................................

Fig(2) scattering of x-rays.....................................................................................................

Fig(3) trigonometric ratio.....................................................................................................

Fig(4) Bragg’s law................................................................................................................

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INTRODUCTION

Microstructure is a very small scale of a material. Analyzing the structure of

material, such as metal, is very crucial to understanding the material’s properties,
state, and influence on other materials. That is why microstructural analysis is vital
in the field of chemistry and mechanics, providing insights into the material’s
mechanical, thermal, and electrical properties. This report talks about the
microstructure of metals specifically and the usage of instruments to analyze the
structural material of metals.

One of the known microstructural methods and instruments to analyze

metals is the usage of x-ray diffraction instrumentation. X-ray diffraction floods
the metal to reveal the arrangement of its atoms. X-ray is suitable for analyzing the
molecular structures of the atoms as it can capture the wavelength of the covalent
bonds between the atoms. The main idea of using x-ray diffraction is analyzing
how the metal reacts to light rays, and from the collected data we predict how the
structure of the atoms looks like.

X-ray diffraction is used for multiple applications including mapping

defects, identifying phases and phases transformation, analyzing residual stress,
and characterizing nanomaterials. This report delves deeper into the geometry and
the physics behind the analysis of the structures using x-ray diffraction.

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HISTORY BEHIND X-RAY DIFFRACTION:
Max von Laue discovered that x-ray could be
diffracted by crystals. His colleagues successfully
obtained the first x-ray diffraction photograph. This
work laid the groundwork for future development,
including Bragg’s law. This law explains the
conditions for constructive interference in crystal
lattices, forming the base for modern x-ray
diffraction analysis. [1]

Kathleen Lonsdale made a breakthrough in the study of biological models.

Lonsdale used x-ray diffraction to determine the structure of a diamond-like
molecule with the formula C6N4H12. This was groundbreaking as it was the first
time a scientist could determine the arrangement of atoms in a complicated
molecule using this technique. [2]

Advancements in x-ray detectors and faster computers that calculated the

microscopic structure of molecules allowed Watson and Crick to analyze the
double helix structure of the DNA.

Nowadays, refinement in instruments and advanced computational power

allows scientists to analyze even smaller and more complex molecules within less
time. For instance, microdiffraction allowed the analysis of specific small regions
of material. [3]

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OBJECTIVES
 Having a physical understanding of x-ray diffraction
 Analyzing the advantages and disadvantages of using XRD
 Studying an experiment
 Understanding the components of the XRD and how they work together.

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HOW XRD WORKS AND ITS PROCESS:

X-ray Diffraction is dependent on the principle of constructive interference of

the X-rays scattered by the crystal lattices. There are 6 key steps.
 First, X-ray generation where a high energy X-ray is emitted usually with a
specific wavelength.
 Second is monochromation in which the
X-ray beams pass through the crystal
monochromator and selecting a
wavelength to increase the diffraction
pattern.
 Third is the incident X-rays now the X-
ray strikes the crystalline sample
Fig(1) x-ray diffraction camera: this figure
according to Bragg’s law the rays go shows how x-ray diffraction cameras usually
through constructive interference when look like [1]

they strike parallel to the planes of atoms

in the crystal lattices.
 Fourth the diffracted X-rays, when the interference results in the specific
angles which the X-rays are diffracted at. Then these diffracted X-rays are
directed into the detector.
 And this brings us to the fifth step which is pattern analysis and it's where
the detector records the intensity and angles of the diffracted X-rays
therefore forming a pattern. This pattern is a unique and it shows the
crystallographic structure of the material.
 Finally, the last step is the Data interpretation, now using the pattern we got
is meant to be analyzed to identify the crystalline phases and the metals
properties and the crystallographic parameter.
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 PHYSICAL VIEW:

An x-ray is an electromagnetic wave that has a

wavelength ranging from 10-11 to 10-8 meters. [1]
When x-rays hit the atoms of the desired material,
they bump into proton, neutron, and electrons of the
atom, causing them to vibrate. Protons and neutrons
vibrate less than electrons. When the rays hit the
electron, the electrons cause the rays to bounce off it
while having almost the same frequency and
wavelength. The rays bounce and scatter in circular
patterns around the electron as shown in figure 1.
The disadvantage of using this technique is that it’s
Fig(2) scattering of x-rays: showing the
harder to study lighter material as they usually have ripple effect created by the beams bouncing
less electrons which causes less scattering. off the electrons [1]

The rays are emitted in specific angles such that the electrons scatter the
waves in constructive interference. This type of scattering is called diffraction. The
angle that forms between the diffracted ray and the incident ray is 2 theta. To get
the distance between the atoms we can use the trigonometric ratio between the
angle, the wavelength, and the distance as shown in figures 3 and 4 [4]

Fig(3) trigonometric ratio: showing the

right triangle formed between the Fig(4) Bragg’s law: showing how the x-rays interact with the
diffracted ray and the atoms atoms and diffract by an angle of 2 theta.

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ADVANTAGES AND DISADVANTAGES:

Of course, every tool has its pros and cons and knowing this will help us reach our
desired result. So, first the pros:
 Phase identification: identifying different crystalline phases which help with
the characterization of its microstructure. [5]

 quantitative analysis: it allows for the quantitative analysis of the phase

composition and providing information of the relative of different
crystallographic phases.

 crystallographic information: shows the crystallographic information (lattice

parameters, crystal size, orientation) resulting in a complete comprehensive
understanding of the material.

But of course, we shouldn't forget the cons of this instrument:

 surface sensitivity: it is primarily a surface- sensitive technique which limits

the ability to see the internal structure of the bulk material.

 sample preparation: to get the most accurate results there is crucial sample
preparation (grinding, proper alignment) which is a bit time consuming.

 limited to crystalline materials: it is the most effective when applied to

crystalline materials, but its accuracy decreases for amorphous or poorly
crystalline substances.

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CONCLUSION:

In conclusion, the discovery of X-ray Diffraction as an important instrument for

microstructure analysis in metals shows its important role in advancing materials
science. From its history with Max von Laue to the modern application, XRD has
become dependable in revealing crystalline structures in metals. The process of
XRD that involves incident and diffracted X-rays, provides a detailed diffraction
pattern, ensuring precise identification of crystalline phases.

The uses of XRD, considering the advantages phase identification, quantitative

analysis, and crystallographic insights, contribute extremely to our understanding
of microstructures. However, knowing its weakness aa surface sensitivity and
sample preparation demands, is essential for researchers who aim to get accurate
and meaningful data. [6]

As we move forward, XRD continues to be an aide for innovation in materials

science, helping in the development of advanced materials with specific properties.
The goal of improving instruments and ensures that XRD remains at the top of
microstructure analysis, shaping the landscape of materials science and preparing
the way for future discoveries in the understanding and engineering of metallic
materials. [7]

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REFERENCES:
[1] X-ray Diffraction and Mineral Analysis – Mineralogy. (n.d.).
https://opengeology.org/Mineralogy/12-x-ray-diffraction-and-mineral-analysis/

[2] Dame Kathleen Lonsdale – Crystallographer | STEM Sisters. (n.d.).

https://www.hmdt.org.uk/hmdtmusic/stemsisters/kathleen-lonsdale-crystallographer/

[3] Harlow, G. S., Lundgren, E., & Escudero‐Escribano, M. (2020, October 1). Recent advances
in surface x-ray diffraction and the potential for determining structure-sensitivity relations in single-
crystal electrocatalysis. Current Opinion in Electrochemistry.
https://doi.org/10.1016/j.coelec.2020.08.005

[4] L. (2023, August 29). Bragg’s Law. Chemistry LibreTexts.

https://chem.libretexts.org/Bookshelves/Analytical_Chemistry/Supplemental_Modules_(Analytic
al_Chemistry)/Instrumentation_and_Analysis/Diffraction_Scattering_Techniques/Bragg’s_Law

[5] Renpu, W. (2011, January 1). Oil and Gas Well Corrosion and Corrosion Prevention. Elsevier
eBooks. https://doi.org/10.1016/b978-0-12-385868-9.00018-x

[6] Surdu, V., & Győrgy, R. (2023, September 4). X-ray Diffraction Data Analysis by Machine
Learning Methods—A Review. Applied Sciences. https://doi.org/10.3390/app13179992

[7] X, S. (2023, December 19). Machine learning sifts through vast data from X-ray diffraction
techniques to find new materials. https://phys.org/news/2023-12-machine-sifts-vast-x-ray-
diffraction.html

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