Issue 29, 2025

Wet-chemical approach to the synthesis of iron whitlockite (Ca18Fe2(HPO4)2(PO4)12) via a dissolution–precipitation process under hydrothermal conditions

Abstract

In the present work, iron whitlockite (Fe-WH, Ca18Fe2(HPO4)2(PO4)12) powder was successfully synthesized by a wet-chemical approach. The synthesis was performed through a dissolution–precipitation process under hydrothermal conditions. The final product was obtained in a time-efficient manner via a phase conversion from CaHPO4·2H2O at 230 °C in just 1 h. Structural properties of the obtained material were comprehensively characterized by X-ray diffraction analysis and FTIR, Raman, and EPR spectroscopy. It was determined that in the as-prepared material, Fe ions mainly exist in a reduced divalent state in accordance with the peculiarities of the WH crystal structure. Magnetic studies also revealed paramagnetic behavior of Fe-WH in the temperature range from 5 to 300 K. Upon annealing, the Fe-WH structure decomposed, forming Fe-doped β-Ca3(PO4)2 and Ca2P2O7. Thermally induced decomposition was accompanied by the oxidation of Fe2+ to Fe3+. The biocompatibility of the synthesized material was assessed by in vitro cytotoxicity experiments with the MC3T3-E1 preosteoblastic cell line. The investigated Fe-WH powder did not show a cytotoxic effect on the cells at all studied concentrations, demonstrating its high biocompatibility.

Graphical abstract: Wet-chemical approach to the synthesis of iron whitlockite (Ca18Fe2(HPO4)2(PO4)12) via a dissolution–precipitation process under hydrothermal conditions

Supplementary files

Article information

Article type
Paper
Submitted
26 Feb 2025
Accepted
15 Jun 2025
First published
16 Jun 2025
This article is Open Access
Creative Commons BY license

CrystEngComm, 2025,27, 4947-4955

Wet-chemical approach to the synthesis of iron whitlockite (Ca18Fe2(HPO4)2(PO4)12) via a dissolution–precipitation process under hydrothermal conditions

D. Griesiute, J. Stadulis, A. Kizalaite, A. Antuzevics, A. Dubnika, D. Zakutna, V. Tyrpekl, C. Su, H. Fang and A. Zarkov, CrystEngComm, 2025, 27, 4947 DOI: 10.1039/D5CE00207A

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