Upload
ahmed-hashem-abdelmohsen
View
246
Download
2
Embed Size (px)
Citation preview
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
By/Ahmed Abdelmohsen
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
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
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
By/Ahmed Abdelmohsen
4- 3D- Bravais Lattice
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
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
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
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.
By/Ahmed Abdelmohsen
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)
By/Ahmed Abdelmohsen
Two factors affecting peak intensity
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
By/Ahmed Abdelmohsen
M
L
K
Kβ x-ray
Kα x-ray
X-ray
Powder Sample
By/Ahmed Abdelmohsen
Cu Kα = 1.54 oA
Cu Kα = 0.71 oA
http://hyperphysics.phy-astr.gsu.edu/
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
By/Ahmed Abdelmohsen
Types X-Ray Diffraction Techniques
9-Single Crystal X-Ray Diffraction
10-X-Ray Powder Diffraction
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
By/Ahmed Abdelmohsen
Indexing – Determination of the unit cell dimensions
By/Ahmed Abdelmohsen
Packing of H-KUAST
Packing of MFU-2
Computer Software for data analysis:
By/Ahmed Abdelmohsen
10- X-Ray Powder Diffraction
XRD Lab- Egypt
http://pubs.usgs.gov/
By/Ahmed Abdelmohsen
By/Ahmed Abdelmohsen
Synthesized by/ Ahmed Abdelmohsen
By/Ahmed Abdelmohsen
By/Ahmed Abdelmohsen
1-Determine d-spaces using software
11- XRD and HRTM Diffraction pattern
By/Ahmed Abdelmohsen
2- Select appropriate (hkl) relating to d-spaces
By/Ahmed Abdelmohsen
3- calculate angles between different (hkl) with relating d-values
By/Ahmed Abdelmohsen
4- Finally, matching the (hkl) values with patterns as shown in:
2.64 o A1.64
oA 1.39 o A
By/Ahmed Abdelmohsen
By/Ahmed Abdelmohsen
Dedication
By/Ahmed Abdelmohsen
[email protected]://www.facebook.com/Ahmed.BaioumyAlfazary