10.

X-ray Diffraction
Question

“How do we measure crystallographic features of

materials?

2
Learning objectives
• Explain the principles of X-ray diffraction
• Perform calculations using Bragg’s law

3
Characterization of Microstructures

For various reasons we need to examine the

microstructure of the materials we manufacture:
• For purposes of quality control – e.g. correct
grain size, phase content, defect content
• For purposes of assessing why a material failed
in a particular application – e.g. correct grain
size, phase content, defect content

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Scale of materials

Relevant Range for Engineering

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How small can we see –
resolution?
• Human eye (unaided) ~ 0.1*10-3 m
• Light microscope ~ 0.5*10-6 m
• limited by wavelength of visible light
• Electron microscopes ~ 1*10-9 m
• Scale of molecules and atoms

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Electromagnetic Waves

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Microscopy

Engineering
and Scientific
Research

Manufacturin
g and Failure
Analysis

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Some Examples

SEM photomicrograph of Ni-based superalloy showing g-g’microstructure. The

The g’ precipitates appear as the darker grey, block-like structures; the g phase
appears as the continuous light grey phase encasing the g’-Ni3(Al-Ti)
precipitates; the carbides (Cr-Mo-W – carbides) appear as the elongated light
grey precipitates. Desired microstructure obtained after casting and heat
treatment.

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 Some Examples

Optical Image of Failure CT blade

– F indicates region of fatigue
failure, R region of over load
failure

If we don’t get it right the

consequences can be
SEM Image of Oxide Defect catastrophic leading to loss of life
responsible for blade failure

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Characterization of Chemistry

Like for microstructure, for various

reasons we need to examine the
chemistry of the materials we
manufacture:
• For purposes of quality control
• Core (alloy) content ranges
• Trace element content

• For purposes of assessing why a

material failed
• Core (alloy) content ranges
• Trace element content

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Quantification of Chemistry

There are various analytical methods

available. The techniques include:
• Energy Dispersion X-ray Spectroscopy (EDX)
• Wavelength Dispersion X-Ray Spectroscopy (WDX)
• X-ray Diffraction (XRD)
• Mass Spectroscopy
• …

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 Some examples

Cast shop Spectrometer for

Metal Analysis – used for Portable Spectrometer for
primary feedstock and primary Metal Analysis – used for scrap
ingot quality control (revert) assessment

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Some examples

SEM with EDX analyzer attached to Vacuum Chamber – used for

failure investigation and for research

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How does X-ray Diffraction work
Unit Cell Building Blocks

BCC
FCC

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X-Ray Diffraction and Crystals

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 X-Ray Diffraction
• Diffraction occurs when a wave encounters a series of regularly spaced
obstacles that
(1) are capable of scattering the wave
(2) have spacings that are comparable in the magnitude to the wavelength

Diffracted beam –
reinforced amplitude

Other extreme –
destructive interference

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X-Ray Diffraction

A
A

B B

Path difference = SQ + QT = 2 x dhkl sin

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Bragg’s Law
n  2d sin
Condition for constructive
interference

•  = wavelength of X-ray
• n = order of reflection (1,2,3,
…)
• d = dhkl = spacing between the
planes
•  = angle between the X-rays
and the plane of interest
• dhkl = distance between parallel
(hkl) planes for cubic systems

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Crystallographic Planes

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Lattice Spacing
a
d hkl 
h 
1
2
k l
2 2 2

• (hkl) are the Miller

indices
• a = lattice parameter

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Diffractometer

λ = 0.155 nm

diffraction pattern for a-iron (BCC)

2θ=45 2θ=83
2θ=65

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Example Problem

• Question : For BCC Fe calculate for the (110), (200), and (211) planes:
• a) interplanar spacing
0.2866
• b) diffraction angle (2) d hkl  nm
h 
1
(a) 2
k l
2 2 2

• Assuming
• lattice parameter a = 0.2866 nm n
•  = 0.155 nm
(b) sin  
2d hkl
• n =1

h k l d sin(θ) θ 2θ

1 1 0 0.2027 0.3824 22.5 45

2 0 0 0.1433 0.5408 32.7 65.4

2 1 1 0.1170 0.6623 41.5 83

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Diffractometer

λ = 0.155 nm

diffraction pattern for a-iron (BCC)

2θ=45 2θ=83
2θ=65

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Diffraction-based Measurements of Residual Stress


• Determination of strain
follows from the
measurement of shifts in Lattice
planes
the position for a given stretch
Bragg peak vs. “strain- Lattice
free” reference: planes
contract

Tensile Compressive
shift shift

sin 0 Intensity
 1
sin  2

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Question

“How do we measure crystallographic features of

materials?

26
Learning objectives
• Explain the principles of X-ray diffraction
• Perform calculations using Bragg’s law

27
Problem 3.67
Determine the expected diffraction angle for the first-
order reflection from the (310) set of planes for BCC
chromium (Cr) when monochromatic radiation of
wavelength 0.0711 nm is used.

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