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Challenges of quantitative phase analysis of iron and steel slags: a look at sample complexity

Published online by Cambridge University Press:  26 May 2023

Jessica E. Lyza Open the ORCID record for Jessica E. Lyza [Opens in a new window] ,
Timothy G. Fawcett Open the ORCID record for Timothy G. Fawcett [Opens in a new window] ,
Sarah N. Page  and
Kelly L. Cook Open the ORCID record for Kelly L. Cook [Opens in a new window]
Jessica E. Lyza*
Affiliation:
Levy Technical Laboratories, Edw. C. Levy Co., Portage, IN, USA
Timothy G. Fawcett
Affiliation:
International Centre for Diffraction Data, Newtown Square, PA, USA
Sarah N. Page
Affiliation:
Levy Technical Laboratories, Edw. C. Levy Co., Portage, IN, USA
Kelly L. Cook
Affiliation:
Levy Technical Laboratories, Edw. C. Levy Co., Portage, IN, USA
*
a)Author to whom correspondence should be addressed. Electronic mail: jlyza@edwclevy.net
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Abstract

Quantitative phase analysis (QPA) of slags is complex due to the natural richness of phases and variability in sample composition. The number of phases frequently exceeds 10, with certain slag types (EAF, BOF, blends, stainless) having extreme peak overlap, making identification difficult. Another convolution arises from the variable crystallite sizes of phases found in slag, as well as the mixture of crystalline and amorphous components specific to each slag type. Additionally, polymorphs are common because of the complexity of the steelmaking and slag cooling processes, such as the cation-doped calcium aluminum silicate (Ca3Al2O6, C3A, Z = 24) supercell in LMF slag. References for these doped variants may not exist or in many cases are not known in advance, therefore it is incumbent on the analyzer to be aware of such discrepancies and choose the best available reference. All issues can compound to form a highly intricate QPA and have prevented previous methods of QPA from accurately measuring phase components in slag. QPA was performed via the internal standard method using 8 wt% ZnO as the internal standard and JADE Pro's Whole Pattern Fitting analysis. For each phase, five variables (lattice parameters, preferred orientation, scale factor, temperature factor, and crystallite size) must be accounted for during quantitation, with a specific emphasis on not refining crystallite sizes for iron oxides and trace phases as they are inclined to over-broaden and interact with the background to improve the goodness of fit (R/E value). Preliminary investigations show somewhat reliable results with the use of custom file sets created within PDF-4+ specifically targeted toward slag minerals to further regulate and normalize the analysis process. The objective of this research is to provide a standard protocol for collecting data, as well as to update methodologies and databases for QPA, to the slag community for implementation in a conventional laboratory setting. Currently, Whole Pattern Fitting “Modified” Rietveld block refinement coupled with the addition of a ZnO internal standard gives the most accurate QPA results, though further research is needed to improve upon the complex issues found in this study of the QPA of slags.

Keywords

slagiron slagsteel slagphase identificationquantitative phase analysis
Type
Proceedings Paper
Information
Powder Diffraction , Volume 38 , Issue 2 , June 2023 , pp. 119 - 138
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Copyright
Copyright © The Author(s), 2023. Published by Cambridge University Press on behalf of International Centre for Diffraction Data

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