Description and survey of methodologies for the determination of amorphous content via X-ray powder diffraction
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Ian C. Madsen
Abstract
The presence of amorphous materials in crystalline samples is an increasingly important issue for diffractionists. Traditional phase quantification via the Rietveld method fails to take into account the occurrence of amorphous material in the sample and without careful attention on behalf of the operator its presence would remain undetected. Awareness of this issue is increasing in importance with the advent of nanotechnology and the blurring of the boundaries between amorphous and crystalline species.
The methodology of a number of different approaches to the determination of amorphous content via X-ray diffraction and an assessment of their performance, is described. Laboratory-based, X-ray diffraction data from a suite of synthetic samples, with amorphous content rangäing from 0.0 to 50 wt%, has been analysed using both direct (in which the contribution of the amorphous component to the pattern is used to obtain an estimate of concentration) and indirect (where the absolute abundances of the crystalline components are used to estimate the amorphous content by difference) methodologies. In addition, both single peak and whole pattern methodologies have been assessed.
All methods produce reasonable results, however the study highlights some of the strengths, deficiencies and applicability of each of the approaches.
© by Oldenbourg Wissenschaftsverlag, Clayton South 3169, Victoria, Germany
Artikel in diesem Heft
- Preface: Modern Rietveld Analysis
- Preface: Modern Rietveld Analysis
- Obtaining models suitable for Rietveld refinement: the EXPO2011 techniques
- Complex inorganic structures from powder diffraction:case of tetrahydroborates of light metals
- Recent developments targeting new and experienced users in EXPGUI, an open source Rietveld analysis interface
- Testing different methods for estimating uncertainties on Rietveld refined parameters using SrRietveld
- Understanding anisotropic microstrain broadening in Rietveld refinement
- On the modelling of the powder pattern from a nanocrystalline material
- Rietveld refinement of energy-dispersive synchrotron measurements
- Description and survey of methodologies for the determination of amorphous content via X-ray powder diffraction
- A case study of parameterized Rietveld refinement:The structural phase transition of CuInSe2
Artikel in diesem Heft
- Preface: Modern Rietveld Analysis
- Preface: Modern Rietveld Analysis
- Obtaining models suitable for Rietveld refinement: the EXPO2011 techniques
- Complex inorganic structures from powder diffraction:case of tetrahydroborates of light metals
- Recent developments targeting new and experienced users in EXPGUI, an open source Rietveld analysis interface
- Testing different methods for estimating uncertainties on Rietveld refined parameters using SrRietveld
- Understanding anisotropic microstrain broadening in Rietveld refinement
- On the modelling of the powder pattern from a nanocrystalline material
- Rietveld refinement of energy-dispersive synchrotron measurements
- Description and survey of methodologies for the determination of amorphous content via X-ray powder diffraction
- A case study of parameterized Rietveld refinement:The structural phase transition of CuInSe2
