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L05 XRD2

The document provides an overview of X-ray diffraction (XRD) techniques used in materials characterization, including the Laue, rotating-crystal, and powder methods. It explains the principles of coherent and incoherent scattering, Bragg's Law, and the use of various X-ray detectors. The document emphasizes the significance of diffraction patterns in identifying crystal structures and material properties.

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tanmay rahman
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7 views17 pages

L05 XRD2

The document provides an overview of X-ray diffraction (XRD) techniques used in materials characterization, including the Laue, rotating-crystal, and powder methods. It explains the principles of coherent and incoherent scattering, Bragg's Law, and the use of various X-ray detectors. The document emphasizes the significance of diffraction patterns in identifying crystal structures and material properties.

Uploaded by

tanmay rahman
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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MATL 5200/6200

Materials Characterization

XRD
- Diffraction of X-ray Beam -

Auburn University Materials Engineering


When X-rays encounter matter,

Auburn University Materials Engineering


Diffraction Patterns
Crystal
Intensity →

Schematic of difference between


the diffraction patterns of various
phases

Sharp peaks

0 90 180 Monoatomic gas


Diffraction angle (2θ) →
No peak

Intensity →
Intensity →

Liquid / Amorphous solid

0 90 180
Diffuse Peak Diffraction angle (2θ) →

Diffraction angle (2θ) →

0 Auburn 90
University Materials Engineering
X-Ray Diffraction
 We can use a monochromatic beam to characterize our
materials. Here, we observe how the x-rays interact with the
material:
• Scattered coherently, reflected/diffracted
• Scattered incoherently,
• Absorbed, and
• Transmitted

 Diffraction occurs when each object in a periodic array


scatters radiation coherently, producing concerted
constructive interference at specific angles.

 Since crystalline substances consist of parallel rows of atoms


separated by a ‘unique’ distance, x-rays can be diffracted off
of them.

Auburn University Materials Engineering


Diffraction from a Crystal

April 1912, von Laue,


Friedrich and
Knippinghad performed
their pioneering
experiment on copper
sulfate.

Auburn University Materials Engineering


X-Ray Diffraction
Coherent Scattering

Auburn University Materials Engineering


X-Ray Diffraction
Incoherent Scattering

Auburn University Materials Engineering


X-Ray Diffraction

nλ = 2d hkl sin θ

 Bragg’s Law can be simply obtained by calculating the path


differences between the two beams above for diffraction.
 The path difference depends on the incident angle (θ) and spacing
between the parallel crystal planes(d). In order to keep these beams
in phase, their path difference (SQ + QT = 2d sinθ) has to equal one or
multiple X-ray wavelengths (nλ).
Auburn University Materials Engineering
Auburn University Materials Engineering
Laue’s Equations
 Bragg’s equation describes diffraction in terms of a scalar equation.
For greatest generality, equations need to describe the diffracted
beam directions in terms of vectors.

• Consider 1D array
of scatterers
spaced “a” apart
• Let x-ray be
incident with
wavelength λ

a ( cos α − cos α o ) =
hλ ,
• In 2D and 3D:
b ( cos α − cos=
α o ) k λ , c ( cos α − cos=
αo ) lλ
The equations must be satisfied simultaneously, it is in general difficult to
produce a diffracted beam with a fixed wavelength and a fixed crystal.

Auburn University Materials Engineering


Diffraction Methods

Laue Method Rotating-crystal Powder Method


Method

Orientation Lattice Constant Lattice Parameters


Single Crystal Single Crystal Poly Crystal
Polychromatic Monchromatic Monchromatic
Fixed Angle Variable Angle Variable Angle

Method Wavelength Angle Specimen


Laue Variable Fixed Single Crystal

Rotating-crystal Fixed Variable (in part) Single Crystal


Powder Fixed Variable Powder

Auburn University Materials Engineering


Laue Method
 Laue Method - used to determine
the orientation of large single
crystals. White radiation is
reflected from, or transmitted
through, a fixed crystal.

 If we placed a polycrystalline
sample in where we have nearly
all possible lattice orientations
we would obtain the following
pattern.

Single Crystal Polycrystalline


Auburn University Materials Engineering
Rotating-Crystal Method
 In the rotating crystal method, a single crystal is
mounted with an axis normal to a monochromatic
x-ray beam. A cylindrical film is placed around it
and the crystal is rotated about the chosen axis.
 As the crystal rotates, sets of lattice planes will at
some point make the correct Bragg angle for the
monochromatic incident beam, and at that point a
diffracted beam will be formed.
 The reflected beams are located on the surface of
imaginary cones. When the film is laid out flat, the
diffraction spots lie on horizontal lines.

Auburn University Materials Engineering


Powder Method
 Both the x-ray tube and the x-ray detector rotate to maintain the
same angle of incidence on either side of the sample.
 For a polycrystalline sample or powder, we have nearly all possible
lattice orientations.

Auburn University Materials Engineering


X-Ray Detectors
Debey-Scherrer Cameras

The DS rings are cross-section of the diffraction cones with the cylindrical surface of
the film. Wet photographic processes, densitometer for reading of intensities

Auburn University Materials Engineering


X-Ray Detectors

 Proportional counter
(most common type)
 X-rays enter the tube and
are absorbed by gas
atoms  the emission of
photoelectrons(electrons
produced by ionization 
collected charge on the
W wire

Auburn University Materials Engineering


X-Ray Detectors
The grid, the anode, the delay lines
and the Xe-CO2 gas mixture are
contained in a sealed vessel with a
beryllium entrance window. In the
conversion region, the incoming X-ray
photons produce primary electrons by
gas ionization. These electrons drift
towards the anode under a high
electric field. The number of electrons is
multiplied in the amplification gap, and
measured by a resistive anode

Auburn University Materials Engineering

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