Selected Topics in X-Ray Diffraction

Under supervision:Professor. H. Karl

Experimental Physics IV

FAME Master Candidate : Ahmed Hashem Baioumy ABDELMOHSENAugsburg University & Grenoble INP

By/Ahmed Abdelmohsen

By/Ahmed Abdelmohsen

Bachelor of Science (Chemistry) - Excellent with first class honor

The prize of the best presenter & best graduation project in faculty of science – Scientific conference

Pre-Master in Materials Science and Nanotechnology - Grade Excellent (Top GPA = A-)

Pre-Master Physical Chemistry

Erasmus Mundus Scholarship – FAME program 2015/2017

Chemist at Central Laboratory, PSAS ,Beni-Suef University

1- Types of Solids2- What is Crystal3- 2D-Bravais Lattice4- 3D- Bravais Lattice5-History of X-Ray6-Electromagnetic Spectrum 7- Production of X-Ray8- How X-Ray Interact With Matter (Bragg’ Law)

9- Single Crystal XRD10- Powder XRD

11- XRD and HRTM Diffraction pattern

TOPICS

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Single Crystal AmorphousPoly-Crystal

Atoms are arranged in a

regular manner

The periodicity of the structure get

interrupted at certain boundaries

The periodicity is completely lost

1- Types of Solids

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2- What is Crystal

Group of Atoms

A lattice is infinite regular arrangement of points (lattice sites) in a vector space.

http://www.physics-in-a-nutshell.com/

Know first what is lattice

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3- 2D-Bravais Lattice

An infinite array of discrete points in generated by a set of discrete translation operation:

1 – oblique 2 – rectangular 3 – centered rectangular

4 – hexagonal (rhombic) 5 – square

Interatomic Distances

Angles

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4- 3D- Bravais Lattice

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X-Ray Diffraction Technique

Non-destructive analytical technique used for the determination of crystallinity of materials by relating the resulting data to more than 70.000 reference card in ICCD

The International Centre for Diffraction Data

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Discovering By The German physicist Roentgen in 1895

Named X-Ray because their nature was unknown at the timeNomenclature

5-History of X-Ray

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X-rays are electromagnetic radiation of exactly the same nature as light but of very much shorter wavelength.

6-Electromagnetic Spectrum

http://hubblesite.org

Wave length ≤ Materials interatomic Distance To be able to determine interatomic distance and angles

Type of Electromagnetic radiation with a

wavelength ranging from 0.01 to 10

nanometers, corresponding to frequencies in the

range 30 petahertz to 30 exahertz(3×1016 Hz

to 3×1019 Hz)

What is X ray

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Anode

Cathode

Electron Beam

X-Ray emission

Cathode Arm

(Tungsten Filament)

7- Production of X-Ray:

By applying high voltage between

electrodes

At a tube voltage of 30,000 volts, this

velocity is about one-third

of light velocity.

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8- How X-Ray Interact With Matter (Bragg’s Law)

2ϴ

ϴ

d

1- The angle of incidence = angle of scattering.2- The pathlength difference is equal to an integer number of wavelengths.

1

2

A C

B

A

D

B

D

ϴdhkl

AB= dhkl sinϴ

2 AB = n (Wave length)

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Two factors affecting peak intensity

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The stronger it scatters X-rays.

Generally, the heavier an element

The more electrons it has

Two factors affecting peak intensity1- Atomic number of the atoms

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M

L

K

Kβ x-ray

Kα x-ray

X-ray

Powder Sample

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Cu Kα = 1.54 oA

Cu Kα = 0.71 oA

http://hyperphysics.phy-astr.gsu.edu/

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Two factors affecting peak intensity2-Orientation of the particles in a powdered sample

http://www.ammrf.org.au/

DOI: 10.1039/C2NR11767CSynthesized by/ Ahmed Abdelmohsen

By/Ahmed Abdelmohsen

Types X-Ray Diffraction Techniques

9-Single Crystal X-Ray Diffraction

10-X-Ray Powder Diffraction

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9- Single Crystal X-Ray Diffraction

Preparation of the sample for measurement:

1-Cut and Pick up one crystal under optical

microscope.

(Few micro-meter)

2- Oil : Paratone oil - Mineral oil

keep air sensitive compounds/Good adhesion/Minimize absorption effect.3- Mounting

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Indexing – Determination of the unit cell dimensions

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Packing of H-KUAST

Packing of MFU-2

Computer Software for data analysis:

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10- X-Ray Powder Diffraction

XRD Lab- Egypt

http://pubs.usgs.gov/

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Synthesized by/ Ahmed Abdelmohsen

By/Ahmed Abdelmohsen

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1-Determine d-spaces using software

11- XRD and HRTM Diffraction pattern

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2- Select appropriate (hkl) relating to d-spaces

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3- calculate angles between different (hkl) with relating d-values

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4- Finally, matching the (hkl) values with patterns as shown in:

2.64 o A1.64

oA 1.39 o A

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Dedication

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Ahmed.h.abdelmohsen@gmail.comhttps://www.facebook.com/Ahmed.BaioumyAlfazary