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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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References

REFERENCES

Association for Iron and Steel Technology. 2022. Steel Glossary. AIST Steel Glossary. http://apps.aist.org/asp/glossary/.Google Scholar
ASTM C702/C702M-18. 2018. Standard Practice for Reducing Samples of Aggregate to Testing Size. West Conshohocken, PA: ASTM International. doi:10.1520/C0702-98R03.Google Scholar
ASTM D75/D75M-19. 2019. Standard Practice for Sampling Aggregates. West Conshohocken, PA: ASTM International. doi:10.1520/D0075_D0075M-19.Google Scholar
ASTM D8021-20. 2021. Standard Guide for Blast Furnace and Steel Furnace Slag as Produced During the Manufacture of Iron and Steel. West Conshohocken, PA: ASTM International. doi:10.1520/D8021-20.Google Scholar
ASTM D8-22. 2022. Standard Terminology Relating to Materials for Roads and Pavement. West Conshohocken, PA: ASTM International. doi:10.1520/D0008-22A.Google Scholar
Congressional Research Services. 2021. “U.S. Steel Manufacturing: National Security and Tariffs.” https://crsreports.congress.gov/product/pdf/IF/IF11897.Google Scholar
Fawcett, T. G., Kabekkodu, S. N., Blanton, J. R., Crowder, C. E., and Blanton, T. N.. 2015. “Simulation Tools and References for the Analysis of Nanomaterials.” Advances in X-ray Analysis 58: 108–20.Google Scholar
Fawcett, T. G., Gates-Rector, S., Gindhart, A. M., Rost, M., Kabekkodu, S. N., Blanton, J. R., and Blanton, T. N.. 2020. “Total Pattern Analyses for Non-Crystalline Materials.” Powder Diffraction 35 (2): 82–88. doi:10.1017/S0885715620000263.CrossRefGoogle Scholar
Fawcett, T. G., Blanton, J. R., Kabekkodu, S. N., Blanton, T. N., Lyza, J., and Broton, D.. 2022. “Best References for the QPA of Portland Cement.” Powder Diffraction 37 (2): 68–75. doi:10.1017/S0885715622000215.CrossRefGoogle Scholar
Gates-Rector, S., and Blanton, T.. 2019. “The Powder Diffraction File: A Quality Materials Characterization Database.” Powder Diffraction 34 (4): 352–60. doi:10.1017/S0885715619000812.CrossRefGoogle Scholar
Jay, A., and Andrews, K.. 1946. “Note on Oxide Systems Pertaining to Steel-Making Furnace Slags. FeO-MnO, FeO-MgO, CaO-MnO, MgO-MnO.” Journal of Iron and Steel Institute 152: 15–18.Google Scholar
McGannon, H. 1971. The Making, Shaping, and Treating of Steel, 9th ed. Pittsburg, PA: United States Steel Corporation.Google Scholar
MDI. 2023. “Jade.” Computer software. International Centre for Diffraction Data. https://www.icdd.com/mdi-jade/.Google Scholar
Mineral Commodity Summaries. 2021. Iron and Steel. Reston, VA: U.S. Geological Survey, 86–89.Google Scholar
Nishinohara, I., Kase, N., Maruoka, H., Hirai, S., and Hiromi, E.. 2015. “Powder X-ray Diffraction Analysis of Lime-Phase Solid Solution in Converter Slag.” ISIJ International 55 (3): 616–22. doi:10.2355/isijinternational.55.616.CrossRefGoogle Scholar
Pellegrino, J. L. 2000. Energy and Environmental Profile of the Chemicals Industry. United States: U.S. Dept. of Energy. doi:10.2172/1218625.CrossRefGoogle Scholar
Peterson, V. K., Ray, A. S., and Hunter, B. A.. 2006. “A Comparative Study of Rietveld Phase Analysis of Cement Clinker Using Neutron, Laboratory X-Ray, and Synchrotron Data.” Powder Diffraction 21 (1): 12–18. doi:10.1154/1.2040455.CrossRefGoogle Scholar
Piatak, N. M., Parsons, M. B., and Seal, R. R.. 2015. “Characteristics and Environmental Aspects of Slag: A Review.” Applied Geochemistry 57: 236–66. doi:10.1016/j.apgeochem.2014.04.009.CrossRefGoogle Scholar
Pritula, O., Smrčok, L., and Baumgartner, B.. 2003. “On Reproducibility of Rietveld Analysis of Reference Portland Cement Clinkers.” Powder Diffraction 18 (1): 16–22. doi:10.1154/1.1545116.CrossRefGoogle Scholar
Scardi, P., Leoni, M., and Faber, J.. 2006. “Diffraction Line Profile from a Disperse System: A Simple Alternative to Voigtian Profiles.” Powder Diffraction 21 (4): 270–77. doi:10.1154/1.2358359.CrossRefGoogle Scholar
Scarlett, N. V., Madsen, I. C., Cranswick, L. M., Lwin, T., Groleau, E., Stephenson, G., Aylmore, M., and Agron-Olshina, N.. 2002. “Outcomes of the International Union of Crystallography Commission on Powder Diffraction Round Robin on Quantitative Phase Analysis: Samples 2, 3, 4, Synthetic Bauxite, Natural Granodiorite and Pharmaceuticals.” Journal of Applied Crystallography 35 (4): 383–400. doi:10.1107/s0021889802008798.CrossRefGoogle Scholar
Sitepu, H., O'Connor, B. H., and Li, D.. 2005. “Comparative Evaluation of the March and Generalized Spherical Harmonic Preferred Orientation Models Using X-Ray Diffraction Data for Molybdite and Calcite Powders.” Journal of Applied Crystallography 38 (1): 158–67. doi:10.1107/s0021889804031231.CrossRefGoogle Scholar
Walenta, G., and Füllmann, T.. 2004. “Advances in Quantitative XRD Analysis for Clinker, Cements, and Cementitious Additions.” Powder Diffraction 19 (1): 40–44. doi:10.1154/1.1649328.CrossRefGoogle Scholar
World Steel Association. 2020. Steel Industry and Co-Products. Brussels, Belgium: World Steel Association, 1–2.Google Scholar