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Thermally induced crystal phase transitions in Zn–Al layered double hydroxides: zinc and aluminium pathways at various pH values

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Abstract

Due to their lamellar nano-sheet structure, layered double hydroxides (LDH) are known as materials suitable for carrying certain active, functional molecules which can be easily intercalated. The properties of LDHs depend strongly on the synthesis parameters, especially on the pH value of the reaction medium. To gain a thorough understanding of how pH impacts the synthesis outcomes, a range of ZnAl-LDH suspensions were created through a modified method of low supersaturation co-precipitation at different pH levels spanning from 7 to 10. Almost all synthesis routes of LDHs, both direct and indirect, employ some kind of thermal treatment, either during the synthesis or after it, aiming to improve the crystallinity of the products. Accordingly, comprehensive thermogravimetric and dynamic scanning calorimetry assessments were carried out on synthesised samples. For those produced at the lowest and highest pH levels, an analysis of emitted gases was conducted. Extensive microstructure examinations via X-ray powder diffraction (XRD) was performed both before and after thermal treatment. Through XRD analysis, complemented by Fourier transform infrared spectroscopy measurements, the crystal phases within the synthesised ZnAl-LDHs were identified, and the microstructure results were compared to delineate the pathways of thermally induced zinc and aluminium crystal phase transitions relative to the pH of the reaction medium.

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Acknowledgements

The authors are very grateful to Dr. Polona Umek from the Jožef Stefan Institute, Ljubljana, Slovenia for the SEM measurements.

Funding

The authors acknowledge the financial support from the Ministry of Science, Technological Development and Innovations, Republic of Serbia, Programme No. 451-03-47/2023-01/200134 and the Slovenian Research agency (research programme P1-0134). The bilateral cooperation between the Republic of Serbia and the Republic of Slovenia No. BI-RS/20-21-042 as well as from the EUREKA E!13085 CAPTAN project are also acknowledged.

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Authors and Affiliations

  1. University of Novi Sad, Faculty of Technology, Bul. Cara Lazara 1, Novi Sad, 21000, Serbia

    B. Miljević, J. M. van der Bergh, S. Vučetić & J. Ranogajec

  2. University of Ljubljana, Faculty of Chemistry and Chemical Technology, Večna Pot 113, 1000, Ljubljana, Slovenia

    R. Cerc Korošec

  3. Built Environment and Sustainable Technologies (BEST) Research Institute, Liverpool John Moores University, Liverpool, UK

    J. M. van der Bergh

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  1. B. Miljević
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  2. R. Cerc Korošec
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  3. J. M. van der Bergh
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  4. S. Vučetić
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  5. J. Ranogajec
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Contributions

Conceptualisation: BM, RCK, JR; Methodology: BM, RCK, JR, SV; Formal analysis and investigation: BM, RCK, JMvdB, SV; Writing—original draft preparation: BM, RCK; Writing—review and editing: JR, JMvdB, SV; Funding acquisition: JR, RCK, SV; Resources: JR, RCK, SV; Supervision: JR.

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Correspondence to B. Miljević.

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Miljević, B., Cerc Korošec, R., van der Bergh, J.M. et al. Thermally induced crystal phase transitions in Zn–Al layered double hydroxides: zinc and aluminium pathways at various pH values. J Therm Anal Calorim (2024). https://doi.org/10.1007/s10973-024-13166-9

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