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PXRD Intro

The document outlines a course on X-ray powder diffraction (XRPD) for the structural characterization of polycrystalline materials. It covers qualitative and quantitative analysis, structural refinement techniques, and compares powder diffraction to single crystal methods. Key information derived from XRPD includes peak positions, intensities, and shapes, which provide insights into crystal systems, unit cell sizes, and material defects.

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54 views10 pages

PXRD Intro

The document outlines a course on X-ray powder diffraction (XRPD) for the structural characterization of polycrystalline materials. It covers qualitative and quantitative analysis, structural refinement techniques, and compares powder diffraction to single crystal methods. Key information derived from XRPD includes peak positions, intensities, and shapes, which provide insights into crystal systems, unit cell sizes, and material defects.

Uploaded by

oandac
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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06541

X-RAY POWDER
DIFFRACTION: STRUCTURAL
CHARACTERISATION OF
POLYCRYSTALLINE
MATERIALS

M Grazia Francesconi
Reading List
In the BJ Library:
1. Solid-State Chemistry and its Applications, AR West,
Chapters 5 & 6

2. Inorganic Materials Chemistry, MT Weller, Chapters 1 & 2

3. X-ray Diffraction Procedures for Polycrystalline


and Amorphous Materials, L Alexander, HP Klug

4. Introduction to X-Ray Powder Diffractometry, R Jenkins,


RL Snyder

[Link]
Outline of the Course

1. Uses and information from powder x-ray


diffraction

2. Qualitative analysis

3. Quantitative analysis

4. Structural Refinement
Uses of x-ray powder
diffraction (XRPD)
X-ray powder diffraction is the most powerful structural
characterisation technique for polycrystalline solids

Qualitative analysis: Phase identification

Quantitative analysis: Determination of cell symmetry and


cell parameters

Structural Refinement: Rietveld Method

Structural Solution: Reciprocal Space Methods,


Real Space Methods
Powder vs single crystal

SIngle crystal - The experiment


Put a crystal in the beam, observe what reflections
come out at what angles for what orientations of the crystal
with what intensities.

Advantages Provides best data for structure solution

Disadvantages Single crystals often difficult to obtain


Single crystals not representative of the bulk
Powder vs single crystal
Powder - The experiment
Samples consists of a collection of many small crystallites with
random orientations
Average over crystal orientations and measure the scattered
intensity as a function of outgoing angle

Disadvantage
Inversion of the measured intensities to find the structure is
more difficult and less reliable

Advantages
Easier to prepare a powder sample
All reflections from all phases in the sample
The experiment: The
diffractometer
The diffractogram I
The intensity I is represented by
a delta functions
(perfectly sharp scattering).

The peaks are broadened

I is a continuous,
slowly varying function
The diffractogram II
(301)
(310)
Intensity

(611) (321)
(600) (411) (002)
(200) (110) (400)

2θ degrees
Pattern - a plot of diffracted intensities vs. angle of diffraction 2θ

dhkl
Peak observed for every plane
fullfilling Bragg’s law
d''h''k''l''
(h,k,l) = Miller Indices
d'h'k'l'
Information from PXRD

1) Peak Positions
(a) Crystal system
(b) Unit Cell Size (Lattice Constants)

2) Peak Intensities
(a) Unit Cell Contents (Atomic Positions, etc.)
(b) Quantitative Phase Determination

3) Peak Shapes
(a) Crystallite Size
(b) Non-uniform Strain
(c) Extended Defects

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