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Thermal transition analysis of fish scale originated hydroxyapatite: AFM and electrochemical impedance spectroscopy as complimentary techniques

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Abstract

Several studies are reported on extraction and characterization of hydroxyapatite (HAp) from biological sources by heat sintering method; however, conversing observations are reported on the optimized sintering conditions and crystalline characteristics of the extracted HAp. The present study systematically depicts the different stages of collagen elimination and crystallization of mineral phase in fish scale occurring during different conditions of heat sintering. The pre-sintering temperature as optimized by thermal analysis by TGA, DTG and DTA curves was at 450 °C. The microcrystalline and structural characteristics of extracted HAp samples were established by SEM, elemental mapping, XRD, FTIR and surface area analysis (BET). Accordingly, complete desorption of residual collagen from scale surface was evidenced at 800 °C, and that from matrix interspace at 900 °C. Stable HAp nanocrystal formation could be achieved at 1000 °C, above which the characteristic features of recrystallization and phase transformation were evident. Hence, 1000 °C was considered as the rate limiting temperature for HAp formation. This could be clearly established by atomic force microscopy (AFM) and electrochemical impedance analysis. Conclusively, the present study established AFM and electrochemical impedance analysis as complimentary techniques to the routine analytical techniques employed in the earlier reports for the confirmation of microstructural alterations and phase transformations occurring in HAp crystals during sintering process.

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Acknowledgements

The authors thank Indian Council for Agricultural Research, ICAR, India for the financial assistance provided to undertake this work.

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Authors and Affiliations

  1. ICAR-Central Institute of Fisheries Technology, Matsyapuri, Willington Island, Cochin, 682 029, India

    P. K. Binsi, P. Muhamed Ashraf & A. A. Zynudheen

  2. Pushpagiri College of Dental Sciences, Perumthuruthy, Kerala, 686 548, India

    Nebu George Thomas

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  1. P. K. Binsi
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  2. P. Muhamed Ashraf
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  4. A. A. Zynudheen
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Correspondence to P. K. Binsi.

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Supplementary Information

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Supplementary figures S1

EDAX spectra of HAp samples extracted at various sintering temperatures for 3 h. A 600-3; B 700-3; C 800-3; D 900-3; E 1000-3; F 1100-3 (PDF 363 KB)

Supplementary file2

Cyclic voltammogram of high and low frequency domain intersection at different temperatures depicting transformation of hydroxyapatite.A 600-3; B 700-3; C 800-3; D 900-3; E 1000-3; F 1100-3 (PDF 229 KB)

Supplementary file3

Electrochemical impedance spectra of HAp samples extracted at various sintering temperatures for 3 h (PDF 134 KB)

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Binsi, P.K., Ashraf, P.M., Thomas, N.G. et al. Thermal transition analysis of fish scale originated hydroxyapatite: AFM and electrochemical impedance spectroscopy as complimentary techniques. J Therm Anal Calorim 147, 4027–4045 (2022). https://doi.org/10.1007/s10973-021-10842-y

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