Lecture 06

Basic Instrumental Techniques
NANO1261
Dr Roshan Thotagamuge
Senior Lecturer
Department of Nano Science Technology, Faculty of
technology, Wayamba University of Sri Lanka.
XRD basics
X-ray diffraction (XRD) uses X-rays to investigate and

quantify the crystalline nature of materials by
measuring the diffraction of X-rays from the planes of
atoms within the material.
It is sensitive to both the type of and relative position
of atoms in the material as well as the length scale
over which the crystalline order persists.
Different disciplines sometimes have different names
for this technique:
• Materials science : XRD (X-ray diffraction)
• Chemistry : PXRD (powder XRD)
• Physics : WAXS (wide angle X-ray scattering)
Nobel prizes for research with X-rays
P. Debye in
W. H. Bragg and W. L. Chemistry for work
Bragg in Physics for on dipole moments
W. C. Roentgen in crystal structure K. M. G. Siegbahn in and diffraction of X
Physics for the derived from X-ray Physics for X-ray rays and electrons in
discovery of X-rays. diffraction. spectroscopy. gases.
1901 1915 1924 1936
1914 1917 1927 1985
M. von Laue in C. G. Barkla in A. H. Compton in H. Hauptman and J.

Physics for X-ray Physics for Physics for discovery Karle in Chemistry
diffraction from characteristic of wavelength for direct methods
crystals. radiation of change in diffused X- to determine X-ray
elements. rays. structures.
Properties
of X-rays
X-rays were discovered in 1895 by German physicist

Roentgen. The typical wavelength of X-rays is 1 x 10-10m (1
angstrom), whereas the wavelength of visible light is typically
1 x 10-6m (1 µm).
X-Ray
• Electromagnetic wave
• High penetrating power
• Very small wave length
Generation of X-rays
X-ray Spectrum from an Iron target
12400
Ø Short Wavelength Limit lSWL (nm) =
V
Ø Continuous spectrum I CS = AiZV m
Ø Characteristic X-ray Moseley’s Law
n = C(Z - s )
I K = Bi (V -V k) n
λSWL
Production of X-rays
X-rays are produced by the deceleration of

charged particles, usually electrons. We
generate X-rays by bombarding a target
material with high energy electrons. The
decelerating electrons produce a
continuous spectrum of energies when
they hit the target called the
‘bremsstrahlung’ which is German for
‘braking radiation’ as it is produced by
stopping electrons.
Diffraction
• A diffracted beam may be defined as a beam composed of a large

number of scattered rays mutually reinforcing each other
Scattering
Interaction with a single particle
Diffraction
Interaction with a crystal
Wave structure
The origin of diffraction is the constructive and

destructive interference of waves. Two waves are said to
be “in phase” if their peaks and troughs are at the same
location. If two waves are in phase, they can sum to
make one wave with a larger amplitude. This is called
constructive interference. If the waves are not in phase
they will sum to make a wave of smaller amplitude, and
this is called destructive interference.
Interaction of X-rays with matter
Scattering Modes
• Random arrangement of atoms in space gives rise to scattering in all

directions: weak effect and intensities add
• By atoms arranged periodically in space
• In a few specific directions satisfying Bragg’s law: strong intensities of the
scattered beam :Diffraction
• No scattering along directions not satisfying Bragg’s law
Young’s Double slit experiment
d sinθ = mλ, m = 1,2,3….. Constructive Interference
d sinθ = (m+½)λ, m = 1,2,3….. Destructive Interference

Interference
Phase Difference = 0˚ Phase Difference = 90˚
Phase Difference = 180˚

Interference and Diffraction
Diffraction of X-rays by a crystal
When an X-ray hits an atom, the X-rays interact with the electron cloud and become scattered in all
directions. The construction below shows that the wave scattered by the lower plane has travelled a
longer distance than the parallel wave scattered by the upper plane. Depending on the angle and the
difference in distance travelled, these waves will sum to give either constructive of destructive
interference.
Diffraction of X-rays by a crystal cont’t.
At certain angles to a crystal plane, the X-rays will constructively interfere (diffract)
and produce a diffracted beam with a much higher intensity that at other angles.
This is described by Bragg's Law:
where n is an integer, λ is the wavelength of the X-rays (in our case 1.54 Å for a
copper tube source), d is the spacing between planes in the atomic lattice of the
sample, and θ is the diffraction angle in degrees.
Diffraction of X-rays by a crystal cont’t.
Diffraction measurements
Diffraction measurements
Anatomy of an X-ray diffractometer - Intro
What the data tells you
What information is actually contained in the diffraction spectra?

Summary of analysis cues
Peak positions show:
• Crystal system
• Space group symmetry
• Translational symmetry
• Unit cell dimensions
• Qualitative phase information
Peak intensities show:

• Unit cell contents
• Point symmetry
• Quantitative phase fractions
Peak shapes and widths show:

• Crystallite size
• Non-uniform microstrain
• Extended defects (stacking faults, antiphase boundaries etc.)
Reality
Crystallite size can be

calculated using
Scherrer Formula
0.9l
t=
B cos q B
Instrumental broadening must be subtracted

(From “Elements of X-ray Diffraction”, B.D. Cullity, Addison Wesley)
Diffractometer
Ø Source
Ø Optics
Ø Detector
Incident Beam Part Diffracted Beam Part
Sample Diffracted Beam

Optics
Source Incident Beam Detector
Optics
Ø Filter to remove Kβ For eg. Ni filter for Cu Kβ
Ø Reduction in intensity of Kα
Ø Choice of proper thickness

Ø Slits To limit the size of beam (Divergence slits)
To alter beam profile

(Soller slit angular divergence )
Ø Narrow slits Lower intensity

+
Narrow peak
Detectors
Ø Single photon detector (Point or 0D)

§ scintillation detector NaI
§ proportional counter, Xenon gas
§ semiconductor
Ø Position sensitive detector (Linear or 1D)

§ gas filled wire detectors, Xenon gas
§ charge coupled devices (CCD)
Ø Area detectors (2D)
§ wire
§ CCD
Ø 3D detector
Photoelectron or Photomultiplier tube or

X-ray photon Electrical signal
Electron-hole pair amplifier
Ø Resolution: ability to distinguish between energies
Ø Energy proportionality: ability to produce signal proportioanl to

energy of x-ray photon detected
Ø Sensitivity: ability to detect low intensity levels
Ø Speed: to capture dynamic phenomenon
Ø Range: better view of the reciprocal space

Data collection and analysis
Ø Choose 2θ range
Ø Step size and time per step
Ø Hardware: slit size, filter, sample alignment
Ø Fast scan followed with a slower scan
Ø Look for fluorescence
Ø Collected data: Background subtraction, Kα2 stripping
Ø Normalize data for comparison I/Imax

Thank you for your attention
Questions? Get in touch:

[email protected]

Lecture 06

Uploaded by

Copyright:

Available Formats

Lecture 06

Uploaded by

Document Information

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Lecture 06

Uploaded by

Copyright:

Available Formats

Basic Instrumental Techniques

X-ray diffraction (XRD) uses X-rays to investigate and

1901 1915 1924 1936

1914 1917 1927 1985

M. von Laue in C. G. Barkla in A. H. Compton in H. Hauptman and J.

X-rays were discovered in 1895 by German physicist

Ø Characteristic X-ray Moseley’s Law

X-rays are produced by the deceleration of

• A diffracted beam may be defined as a beam composed of a large

The origin of diffraction is the constructive and

• Random arrangement of atoms in space gives rise to scattering in all

d sinθ = mλ, m = 1,2,3….. Constructive Interference

d sinθ = (m+½)λ, m = 1,2,3….. Destructive Interference

Phase Difference = 180˚

What information is actually contained in the diffraction spectra?

Peak intensities show:

Peak shapes and widths show:

Crystallite size can be

Instrumental broadening must be subtracted

Incident Beam Part Diffracted Beam Part

Sample Diffracted Beam

Ø Choice of proper thickness

To alter beam profile

Ø Narrow slits Lower intensity

Ø Single photon detector (Point or 0D)

Ø Position sensitive detector (Linear or 1D)

Photoelectron or Photomultiplier tube or

Ø Energy proportionality: ability to produce signal proportioanl to

Ø Sensitivity: ability to detect low intensity levels

Ø Speed: to capture dynamic phenomenon

Ø Range: better view of the reciprocal space

Ø Step size and time per step

Ø Hardware: slit size, filter, sample alignment

Ø Fast scan followed with a slower scan

Ø Look for fluorescence

Ø Collected data: Background subtraction, Kα2 stripping

Ø Normalize data for comparison I/Imax

Questions? Get in touch:

You might also like