Research Data Leeds Repository

Citation

Marsh, Alastair T. M. and Brown, Andrew and Freeman, Helen and Walkley, Brant and Pendlowski, Helen A. and Bernal, Susan A. (2024) Dataset for "Determining aluminium co-ordination of kaolinitic clays before and after calcination with electron energy loss spectroscopy". University of Leeds. [Dataset] https://doi.org/10.5518/1531

Dataset description

Developing a greater understanding of kaolinite dehydroxylation upon calcination is crucial for several industrial applications, including cements. Aluminium coordination in meta-kaolinite indicates the extent of its dehydroxylation and its potential chemical reactivity, and it is typically determined using 27Al magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy. This technique however presents limitations for Fe-rich materials, given the magnetic properties of Fe ions and minerals containing Fe. In this study, the effect of calcination on Al coordination was assessed in a low-Fe clay used as a reference system, and a Fe-rich clay. Al coordination in the low-Fe clay was quantified via 27Al MAS NMR spectra deconvolution, using data collected at 9.4 T and 11.7 T. Energy dispersive X-ray spectroscopy (EDX) maps and electron energy loss spectroscopy (EELS) measurements were carried out in a scanning transmission electron microscope (STEM) on both clays. Al K-edge EEL spectra showed distinguishable 4/5-fold Al and 6-fold Al sites in both clay types. Differences in line-profile indicated a higher proportion of 4/5-fold Al in kaolinite in the Fe-rich clay compared to the low-Fe clay. Conversely, the Fe-rich clay contained a lower proportion of 4/5-fold Al in meta-kaolinite after calcination, relative to the low-Fe clay. These differences are consistent with the greater structural disorder of the meta-kaolinite identified in the Fe-rich clay by X-ray diffraction and the geological origins of both clays. Overall, this study demonstrates the potential of EELS to provide information about Al coordination for individual kaolinite and meta-kaolinite particles.

Keywords:	Monochromated EELS; Low dose TEM; Kaolinite; Metakaolin; Calcined clays; Solid State NMR
Subjects:	J000 - Technologies > J100 - Minerals technology > J140 - Minerals processing
Divisions:	Faculty of Engineering and Physical Sciences > School of Civil Engineering
Related resources:	Location Type https://doi.org/10.1016/j.clay.2024.107402 Publication https://eprints.whiterose.ac.uk/212668/ Publication
License:	Creative Commons Attribution 4.0 International (CC BY 4.0)
Date deposited:	11 Jun 2024 08:11
URI:	https://archive.researchdata.leeds.ac.uk/id/eprint/1295
Additional details Additional details Creators or authors: Creators ORCID Other ID Email Primary affiliation Primary affiliation ID Primary affiliation ID type Secondary affiliation Secondary affiliation ID Secondary affiliation ID type Marsh, Alastair T. M. https://orcid.org/0000-0002-5603-4643 University of Leeds https://ror.org/024mrxd33 ror Brown, Andrew https://orcid.org/0000-0001-9692-2154 University of Leeds https://ror.org/024mrxd33 ror Freeman, Helen https://orcid.org/0000-0001-8242-9561 University of Leeds https://ror.org/024mrxd33 ror Walkley, Brant https://orcid.org/0000-0003-1069-1362 University of Sheffield https://ror.org/05krs5044 ror Pendlowski, Helen A. https://orcid.org/0000-0002-5873-4467 The James Hutton Institute https://ror.org/03rzp5127 ror Bernal, Susan A. https://orcid.org/0000-0002-9647-3106 University of Leeds https://ror.org/024mrxd33 ror Type of data: Dataset Research funders: EPSRC Grant numbers: EP/R001642/1 Publication date: 11 June 2024 Resource language: English Metadata language: English Publisher: University of Leeds Contact email: a.marsh@leeds.ac.uk Last Modified: 03 Sep 2024 10:25

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Data

Dataset for "Determining aluminium co-ordination of kaolinitic clays before and after calcination with electron energy loss spectroscopy" [6MB] Dataset for "Determining aluminium co-ordination of kaolinitic clays before and after calcination with electron energy loss spectroscopy" [6MB] Dataset for "Determining aluminium co-ordination of kaolinitic clays before and after calcination with electron energy loss spectroscopy" [6MB] Security: Anyone File name: ResearchData_2024-05-07.xlsx Content type: Data Description: The data contained in this workbook has been used to create the following figures in the journal article: Marsh, A.T.M., Brown, A.P., Freeman, H.M., Walkley, B., Pendlowski, H., Bernal, S.A. 2024. Determining aluminium co-ordination of kaolinitic clays be Mime-Type: application/vnd.openxmlformats-officedocument.spreadsheetml.sheet License: Creative Commons Attribution 4.0 International (CC BY 4.0) File size: 6MB