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Selected Topics in X-Ray Diffraction Under supervision: Professor. H. Karl Experimental Physics IV FAME Master Candidate : Ahmed Hashem Baioumy ABDELMOHSEN Augsburg University & Grenoble INP By/Ahmed Abdelmohsen

Selected topics in x ray diffrcation ahmed abdelmohsen fame master

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Page 1: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

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

Page 2: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

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

Page 3: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

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

By/Ahmed Abdelmohsen

Page 4: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

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

Page 5: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

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

Page 6: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

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

Page 7: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

4- 3D- Bravais Lattice

Page 8: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

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

Page 9: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

Discovering By The German physicist Roentgen in 1895

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

5-History of X-Ray

Page 10: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

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

Page 11: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

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.

Page 12: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

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

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)

Page 13: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

Two factors affecting peak intensity

Page 14: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

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

Page 15: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

M

L

K

Kβ x-ray

Kα x-ray

X-ray

Powder Sample

Page 16: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

Cu Kα = 1.54 oA

Cu Kα = 0.71 oA

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

Page 17: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

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

Page 18: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

Types X-Ray Diffraction Techniques

9-Single Crystal X-Ray Diffraction

10-X-Ray Powder Diffraction

Page 19: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

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

Page 20: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

Indexing – Determination of the unit cell dimensions

Page 21: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

Packing of H-KUAST

Packing of MFU-2

Computer Software for data analysis:

Page 22: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

10- X-Ray Powder Diffraction

XRD Lab- Egypt

http://pubs.usgs.gov/

Page 23: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

Page 24: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

Synthesized by/ Ahmed Abdelmohsen

Page 25: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

Page 26: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

1-Determine d-spaces using software

11- XRD and HRTM Diffraction pattern

Page 27: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

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

Page 28: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

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

Page 29: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

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

2.64 o A1.64

oA 1.39 o A

Page 30: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

Page 31: Selected topics in x ray diffrcation  ahmed  abdelmohsen  fame master

By/Ahmed Abdelmohsen

Dedication