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Forced hydrolysis of FeCl3 solutions in the presence of Cr3+ ions and hexamethylenetetramine

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  • FOCUS ISSUE: Mössbauer Spectroscopy from Artificial Nano Architectures to Environmental Applications
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Abstract

The phase analysis and nanostructural properties of the precipitates formed by forced hydrolysis of FeCl3 solutions at 160 °C in the presence of Cr3+ ions and hexamethylenetetramine (HMTA) were investigated. The phase analyses of the precipitates showed the presence of ferrihydrite (amorphous-like), α-FeOOH, β-FeOOH, and α-Fe2O3. The exact phase composition was strongly dependent on the starting chemical composition in the solution and the precipitation time. Ferrihydrite, α-FeOOH, and β-FeOOH were the precursors of α-Fe2O3 as the end-product. Upon 2 h of autoclaving at 160 °C, the precipitates consisted of nanoparticles ~ 35 to ~ 50 nm in size, whereas after 24 h their size increased to ~ 100 nm. New shapes of these nanoparticles were found. In these precipitation systems crystalline chromium (hydrous)oxide phase was not detected. However, the formation of solid solutions between Cr3+ ions and iron oxides could not be excluded taking into account Energy-dispersive X-ray spectroscopy (EDS) measurements.

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Acknowledgments

This work was supported by the Croatian Science Foundation (Grant No. IP-2016-06-8254).

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Correspondence to Marko Robić.

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This work was presented at the ACS Fall National Meeting, Atlanta, Georgia, USA, August 22–26 2021.

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Robić, M., Ristić, M., Krehula, S. et al. Forced hydrolysis of FeCl3 solutions in the presence of Cr3+ ions and hexamethylenetetramine. Journal of Materials Research 38, 1048–1060 (2023). https://doi.org/10.1557/s43578-022-00756-2

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