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What Is X-Ray Powder Diffraction (XRD)

X-ray powder diffraction is a technique used to identify crystalline materials by analyzing their diffraction patterns when bombarded with X-rays. The document discusses how XRD works based on Bragg's law, the instrumentation including an X-ray tube, sample holder, and detector, and its applications such as mineral identification and characterization. Strengths are its rapid analysis and unambiguous identification of minerals. Limitations include requiring homogeneous materials and reference patterns for interpretation.

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Ahmad Nawaz
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284 views7 pages

What Is X-Ray Powder Diffraction (XRD)

X-ray powder diffraction is a technique used to identify crystalline materials by analyzing their diffraction patterns when bombarded with X-rays. The document discusses how XRD works based on Bragg's law, the instrumentation including an X-ray tube, sample holder, and detector, and its applications such as mineral identification and characterization. Strengths are its rapid analysis and unambiguous identification of minerals. Limitations include requiring homogeneous materials and reference patterns for interpretation.

Uploaded by

Ahmad Nawaz
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 DOCX, PDF, TXT or read online on Scribd
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X-ray Powder Diffraction (XRD)

Barbara L Dutrow, Louisiana State University


,
Christine M. Clark, Eastern Michigan University

What is X-ray Powder Diffraction (XRD)


X-ray powder diffraction (XRD) is a rapid analytical technique primarily used for phase
identification of a crystalline material and can provide information on unit cell
dimensions. The analyzed material is finely ground, homogenized, and average bulk
composition is determined.

Fundamental Principles of X-ray Powder


Diffraction (XRD)
Max von Laue, in 1912, discovered that crystalline substances act as three-
dimensional diffraction gratings for X-ray wavelengths similar to the spacing of planes
in a crystal lattice. X-ray diffraction is now a common technique for the study of crystal
structures and atomic spacing.
X-ray diffraction is based on constructive interference of monochromatic X-rays and a
crystalline sample. These X-rays are generated by a cathode ray tube, filtered to
produce monochromatic radiation, collimated to concentrate, and directed toward the
sample. The interaction of the incident rays with the sample produces constructive
interference (and a diffracted ray) when conditions satisfy Bragg's Law (nλ=2d sin θ).
This law relates the wavelength of electromagnetic radiation to the diffraction angle
and the lattice spacing in a crystalline sample. These diffracted X-rays are then
detected, processed and counted. By scanning the sample through a range of 2θangles,
all possible diffraction directions of the lattice should be attained due to the random
orientation of the powdered material. Conversion of the diffraction peaks to d-
spacings allows identification of the mineral because each mineral has a set of unique
d-spacings. Typically, this is achieved by comparison of d-spacings with standard
reference patterns.

All diffraction methods are based on generation of X-rays in an X-ray tube. These X-
rays are directed at the sample, and the diffracted rays are collected. A key component
of all diffraction is the angle between the incident and diffracted rays. Powder and
single crystal diffraction vary in instrumentation beyond this.

X-ray Powder Diffraction (XRD)


Instrumentation - How Does It Work?
X-ray diffractometers consist of three basic elements: an X-ray tube, a sample holder,
and an X-ray detector.
Bruker's X-ray Diffraction D8-Discover instrument. Details

X-rays are generated in a cathode ray tube by heating a filament to produce electrons,
accelerating the electrons toward a target by applying a voltage, and bombarding the
target material with electrons. When electrons have sufficient energy to dislodge inner
shell electrons of the target material, characteristic X-ray spectra are produced. These
spectra consist of several components, the most common being Kα and Kβ. Kα consists,
in part, of Kα1 and Kα2. Kα1 has a slightly shorter wavelength and twice the intensity as Kα2.
The specific wavelengths are characteristic of the target material (Cu, Fe, Mo, Cr).
Filtering, by foils or crystal monochrometers, is required to produce monochromatic X-
rays needed for diffraction. Kα1and Kα2 are sufficiently close in wavelength such that a
weighted average of the two is used. Copper is the most common target material for
single-crystal diffraction, with CuKα radiation = 1.5418Å. These X-rays are collimated
and directed onto the sample. As the sample and detector are rotated, the intensity of
the reflected X-rays is recorded. When the geometry of the incident X-rays impinging
the sample satisfies the Bragg Equation, constructive interference occurs and a peak in
intensity occurs. A detector records and processes this X-ray signal and converts the
signal to a count rate which is then output to a device such as a printer or computer
monitor.
Show caption

The geometry of an X-ray diffractometer is such that the sample rotates in the path of
the collimated X-ray beam at an angle θ while the X-ray detector is mounted on an arm
to collect the diffracted X-rays and rotates at an angle of 2θ. The instrument used to
maintain the angle and rotate the sample is termed a goniometer. For typical powder
patterns, data is collected at 2θ from ~5° to 70°, angles that are preset in the X-ray
scan.

Applications
X-ray powder diffraction is most widely used for the identification of unknown
crystalline materials (e.g. minerals, inorganic compounds). Determination of unknown
solids is critical to studies in geology, environmental science, material science,
engineering and biology.
Other applications include:
 characterization of crystalline materials

 identification of fine-grained minerals such as clays and mixed layer clays that
are difficult to determine optically

 determination of unit cell dimensions

 measurement of sample purity

With specialized techniques, XRD can be used to:

 determine crystal structures using Rietveld refinement

 determine of modal amounts of minerals (quantitative analysis)

 characterize thin films samples by:

o determining lattice mismatch between film and substrate and to inferring


stress and strain

o determining dislocation density and quality of the film by rocking curve


measurements

o measuring superlattices in multilayered epitaxial structures

o determining the thickness, roughness and density of the film using glancing
incidence X-ray reflectivity measurements

 make textural measurements, such as the orientation of grains, in a


polycrystalline sample
Strengths and Limitations of X-ray Powder
Diffraction (XRD)?
Strengths
 Powerful and rapid (< 20 min) technique for identification of an unknown mineral

 In most cases, it provides an unambiguous mineral determination

 Minimal sample preparation is required

 XRD units are widely available

 Data interpretation is relatively straight forward

Limitations
 Homogeneous and single phase material is best for identification of an unknown

 Must have access to a standard reference file of inorganic compounds (d-


spacings, hkls)

 Requires tenths of a gram of material which must be ground into a powder

 For mixed materials, detection limit is ~ 2% of sample

 For unit cell determinations, indexing of patterns for non-isometric crystal


systems is complicated
 Peak overlay may occur and worsens for high angle 'reflections'

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