X-RAY DIFFRACTION (XRD)

Principles and Applications

7th February 2023
Dr. Mohamad Alnarabiji
Center for Advanced Materials and Energy
Sciences (CAMES), Universiti Brunei
Darussalam
October 28, 1985
Center For Advanced Materials And Energy Sciences (CAMES)
X-ray was discovered d by WC
Rontgen in 1895
X-ray machine
 Bragg’s Law

Bragg’s law relates the diffraction angle (2θ), to dhkl (a family of

planes produces a diffraction peak only at a specific angle 2θ)
Diffraction of single crystal
Diffraction of polycrystalline sample
Face Centered Centered Cubic Cell Body Centered Centered Cubic Cell

Permitive Primitive Cubic Cell

Miller Indices
 The X-Ray Diffraction Spectrum Ray Diffraction Spectrum

Crystal arrangement

contains information about the

atomic arrangement within the
crystals.
Sum of diffraction patterns
One of the most important uses of XRD:
• Obtain XRD pattern.
• Measure d-spacings.
• Obtain integrated intensities.
• Compare data with known standards in the JCPDS file,
which are for random orientations (there are more than
50,000 JCPDS cards of inorganic materials).
THANK YOU

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“X-RAY PHOTOELECTRON
SPECTROSCOPY (XPS)
What do we mean by surface analysis?
• A surface means different things to different people
• Astronomers- light years for galaxy 10’s km for the suns surface
• Seismologist- km’s – m’s for earth crust
• Builders- m’s – mm’s for surface finish
• Engineers- mm’s to µm’s for surface finish
• Semiconductors (and surface analysts)- µm’s to nm’s

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 So what do these units
mean?
• 1 m = 1000 mm = 103 mm
• 1 m = 1 000 000 µm = 106 mm
• 1 m = 1 000 000 000 nm = 109 nm

• Roughly 1 atomic layer is 0.1 nm

The unit sometimes used is Å (Angstrom) which is 10-10 m

So how thick is a surface analyst?

Generally they are interested in the 0.1 nm to 1 µm range

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 Surface vs. bulk

The surface is the interface between something solid and the atmosphere

Thin films are something which is thin (of the order of atomic sizes) which requires
‘surface analysis’ techniques to see it 7
 Why are we interested in the
surface?
• Simple example
• Problem: Cannot ‘glue’ two pieces of aluminium together
• Aluminium is a reactive metal
Surface analysis
Bulk analysis
(10 nm)
(1 µm) 45at% Oxygen
0.5at% Oxygen 30at.%
99.5at% Aluminium
Aluminium 10at% Carbon
5at% Fluorine
Bulk analysis Presence F
does not tell us if preventing bonding?
something is
preventing Weakly bound carbon
bonding – layer preventing
Oxygen from
bonding?
oxide layer 9
 WHAT IS SURFACE ANALYSIS?
• A type of investigation
performed on the outermost
layer of a solid material.
• Surface analysis is performed by
exciting the surface of a material
using an energy source (primary
beam), and then observing and
analyzing what occurs as a XPS
result of this energization to
determine the properties of a
material's surface.
• Generally requires sophisticated
instruments

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SIMS
 Electrons in Atoms
• Electrons in atoms are found in “shells”
– Each shell is numbered 1, 2, 3..
– Shell 1 is closest to the nucleus
– Each electron orbits around the nucleus
– Each orbit has a well-defined energy
– Electrons nearest the nucleus are most strongly
attracted, and require most energy to remove- they have
a high binding energy
• Electrons in shells form “sub-shells”
– From shell 2, different shapes of orbit occur
– Each different orbit has a different energy
– Orbits are labelled s, p, d, f and are filled with electrons
in that order
– S orbits have higher binding energy than p 17
 Ionization

• XPS process
– An electron is ejected by a photon

– Electron KE = hn - BE
– So photoelectrons have a characteristic binding energy for each element20
XPS – survey spectrum

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 Application

• Example: Catalysis

Lattice O,
O1s FWHM=0.95

Adsorbed O,
FWHM=2.85

TEM micrograph of Cu/ZnO 36

catalyst on CNTs XPS of Cu/ZnO catalyst on CNTs
 Application

• Example: Semiconductor
• Control of thin layer thickness is
critical in semiconductors
• Depth profiles are used to
determine the elemental
composition as a function of
depth.
v There are alternating SiO2 and
non-stoichiometric TaOx layers in
the dielectric film, SiO2 being the
first layer.
v Also, outer layers are thinner
than the inner layers, though the
first SiO2layer is thicker than the
other outer SiO2 layers. XPS depth profile of a 22-layer SiO2 and tantalum
oxide (Ta2O5) dielectric reflective film on the interior
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wall of a hollow quartz material.
Full and narrow scan
THANK YOU

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