X-RAY DIFFRACTOMETER: X-rays is a form of electromagnetic radiation. Xrays have a wavelength in the range of 10 to 0.

01 nanometers, corresponding to frequencies in

the range 30 petahertz to 30 exahertz (3 1016 Hz to 3 1019 Hz) and energies in the range
120 eV to 120 keV. X-rays have shorter wavelengths than ultraviolet light but longer
wavelengths than gamma rays.
a method of determining the arrangement of atoms within a crystal, in which a beam of X-ray
strikes a crystal and diffracts into many specific directions.
this method determined the size of atoms, the lengths and types of chemical bonds, and the
atomic-scale differences among various materials, especially minerals and alloys

A crystal consists of a periodic arrangement of the unit cell into a lattice. The unit cell
can contain a single atom or atoms in a fixed arrangement.
Crystals consist of planes of atoms that are spaced a distance d apart, but can be resolved
into many atomic planes, each with a different d-spacing.
a,b and c (length) and a, b and g angles between a,b and c are lattice constants or
parameters which can be determined by XRD.

Why XRD?
Measure the average spacings between layers or rows of atoms
Determine the orientation of a single crystal or grain
Find the crystal structure of an unknown material
Measure the size, shape and internal stress of small crystalline regions
Specimen Preparation: Double sided tape Glass slide Powders: 0.1mm < particle size
<40 mm Peak broadening less diffraction occurring
Bulks:
smooth surface after polishing, specimens should be thermal annealed to
eliminate any surface deformation induced during polishing.

Braggs law is a simplistic model to understand

what conditions are required for diffraction.

For parallel planes of atoms, with a space dhkl between the planes, constructive
interference only occurs when Braggs law is satisfied.

In our diffractometers, the X-ray wavelength is fixed.

Consequently, a family of planes produces a diffraction peak only at a specific angle .
Additionally, the plane normal must be parallel to the diffraction vector

dhkl dhkl

2d hkl sin

Plane normal: the direction perpendicular to a plane of atoms

Diffraction vector: the vector that bisects the angle between the incident and diffracted beam

The space between diffracting planes of atoms determines peak positions.

The peak intensity is determined by what atoms are in the diffracting plane.

Our powder diffractometers typically use the

Bragg-Brentano geometry.
Detector
X-ray
tube

The incident angle, , is defined between the X-ray source and the sample.
The diffracted angle, 2 , is defined between the incident beam and the
detector angle.
The incident angle is always of the detector angle 2 .
In a :2 instrument (e.g. Rigaku RU300), the tube is fixed, the sample
rotates at /min and the detector rotates at 2 /min.
In a : instrument (e.g. PANalytical XPert Pro), the sample is fixed and the
tube rotates at a rate - /min and the detector rotates at a rate of /min.

The peak position as 2q depends on instrumental characteristics such as wavelength.

The peak position as d hkl is an intrinsic, instrument-independent, material
property.
Braggs Law is used to convert observed 2q positions to dhkl.
The absolute intensity, i.e. the number of X rays observed in a given peak, can vary due
to instrumental and experimental parameters.
The relative intensities of the diffraction peaks should be instrument independent.
To calculate relative intensity, divide the absolute intensity of every peak
by the absolute intensity of the most intense peak, and then convert to a

percentage. The most intense peak of a phase is therefore always called

the 100% peak.
Peak areas are much more reliable than peak heights as a measure of intensity.

Application of XRD:

Phase Composition of a Sample

Quantitative Phase Analysis: determine the relative amounts of phases in a
mixture by referencing the relative peak intensities
Unit cell lattice parameters and Bravais lattice symmetry
Index peak positions
Lattice parameters can vary as a function of, and therefore give you information
about, alloying, doping, solid solutions, strains, etc.
Residual Strain (macrostrain)
Crystal Structure
By Rietveld refinement of the entire diffraction pattern
Epitaxy/Texture/Orientation
Crystallite Size and Microstrain
Indicated by peak broadening
Other defects (stacking faults, etc.) can be measured by analysis of peak shapes
and peak width
We have in-situ capabilities, too (evaluate all properties above as a function of time,
temperature, and gas environment).
Typical applications for XRD include analysis of coal ash, exploration drill cores, mill
circuit head, tail, rougher, and concentrate samplings, power plant corrosion deposits,
boiler tube scale, clay minerals, waste streams, mineral products, crystalline phases in
fused silica, contaminants in tungsten carbide, swelling minerals in soils, and industrial
by-products.
Identification of bulk mineralogy (Silicates, Carbonates, Sulfates, Oxides and etc).
Identification of clay minerals.
Semi-quantitative estimation of clays mineral
Measurement of Illite crystallite in order to estimate thermal maturity
Indirect assessment of level of organic matter maturation by using Illaite crystality data
Determination of Sedimentary environments by using identification and Semiquantitative estimation information and data.
Temperature and time dependent processes determine the conversion of organic matter to
oil and gas and the extent of most digenetic mineral reactions. Thermal history and
maturity reconstructions are, therefore, a key factor for the exploration strategy. Such
simulations become meaningful for exploration purposes if the complex interaction of all
involved factors is analyzed.
Subsidence and burial history of single wells or basins
Down hole mineral and lithotype logs which allow improved calibration and
interpretation of geophysical wireline logs; cross-well correlation; improved source, seal

and reservoir characterization; in-situ heavy mineral provenance studies which preserves
textural context and enhances interpretation.
The resulting high resolution digital images allow classification of cuttings and cores into
quantitative lithotypes. This classification is based on mineralogy and micro-texture.
Suspected cavings can be digitally removed and the data renormalized caving-free.
In-situ XRD allows the laboratory-scale examination of mineral processing reactions
under operating conditions, which is useful in determining reaction mechanisms and
kinetics