Dissolution-precipitation synthesis and thermal stability of magnesium whitlockite

Agne Kizalaite; Vytautas Klimavicius; Vytautas Balevicius; Gediminas Niaura; Andrei N. Salak; Jen Chang Yang; Sung Hun Cho; Tomoyo Goto; Tohru Sekino; Aleksej Zarkov

doi:10.1039/d3ce00602f

Dissolution-precipitation synthesis and thermal stability of magnesium whitlockite

Agne Kizalaite, Vytautas Klimavicius, Vytautas Balevicius, Gediminas Niaura, Andrei N. Salak, Jen Chang Yang, Sung Hun Cho, Tomoyo Goto, Tohru Sekino, Aleksej Zarkov

Research output: Contribution to journal › Article › peer-review

7 Citations (Scopus)

Abstract

Magnesium whitlockite (Mg-WH, Ca₁₈Mg₂(HPO₄)₂(PO₄)₁₂) is a promising candidate for biomedical application in bone regeneration; however, the fabrication of Mg-WH bioceramics by conventional methods is limited. Mg-WH is known to be thermally unstable and decomposes upon heating. The mechanism of thermal decomposition and phase evolution has not comprehensively been investigated so far. In the present work, Mg-WH was synthesized by a dissolution-precipitation process under hydrothermal conditions. Thermally induced degradation of the synthesized powders was investigated in detail by combining X-ray diffraction (XRD) analysis, infrared spectroscopy (FTIR), Raman spectroscopy as well as ¹H and ³¹P solid-state nuclear magnetic resonance (NMR). The as-prepared Mg-WH powders were annealed at different temperatures in the range from 400 to 1300 °C. It was found that thermal decomposition starts at around 700 °C with the formation of beta-tricalcium phosphate (β-TCP, Ca₃(PO₄)₂) and a mixture of two Ca₂P₂O₇ polymorphs. Thermal decomposition occurs gradually and the co-existence of both Mg-WH and Mg-substituted β-TCP phases was observed in a wide temperature range up to 1200 °C. Complete disappearance of the HPO₄²⁻ structural unit was confirmed only after annealing at 1300 °C followed by melting at 1400 °C.

Original language	English
Pages (from-to)	4370-4379
Number of pages	10
Journal	CrystEngComm
Volume	25
Issue number	30
DOIs	https://doi.org/10.1039/d3ce00602f
Publication status	Published - Jul 10 2023

ASJC Scopus subject areas

General Chemistry
General Materials Science
Condensed Matter Physics

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title = "Dissolution-precipitation synthesis and thermal stability of magnesium whitlockite",

abstract = "Magnesium whitlockite (Mg-WH, Ca18Mg2(HPO4)2(PO4)12) is a promising candidate for biomedical application in bone regeneration; however, the fabrication of Mg-WH bioceramics by conventional methods is limited. Mg-WH is known to be thermally unstable and decomposes upon heating. The mechanism of thermal decomposition and phase evolution has not comprehensively been investigated so far. In the present work, Mg-WH was synthesized by a dissolution-precipitation process under hydrothermal conditions. Thermally induced degradation of the synthesized powders was investigated in detail by combining X-ray diffraction (XRD) analysis, infrared spectroscopy (FTIR), Raman spectroscopy as well as 1H and 31P solid-state nuclear magnetic resonance (NMR). The as-prepared Mg-WH powders were annealed at different temperatures in the range from 400 to 1300 °C. It was found that thermal decomposition starts at around 700 °C with the formation of beta-tricalcium phosphate (β-TCP, Ca3(PO4)2) and a mixture of two Ca2P2O7 polymorphs. Thermal decomposition occurs gradually and the co-existence of both Mg-WH and Mg-substituted β-TCP phases was observed in a wide temperature range up to 1200 °C. Complete disappearance of the HPO42− structural unit was confirmed only after annealing at 1300 °C followed by melting at 1400 °C.",

author = "Agne Kizalaite and Vytautas Klimavicius and Vytautas Balevicius and Gediminas Niaura and Salak, {Andrei N.} and Yang, {Jen Chang} and Cho, {Sung Hun} and Tomoyo Goto and Tohru Sekino and Aleksej Zarkov",

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AU - Kizalaite, Agne

AU - Klimavicius, Vytautas

AU - Balevicius, Vytautas

AU - Niaura, Gediminas

AU - Salak, Andrei N.

AU - Yang, Jen Chang

AU - Cho, Sung Hun

AU - Goto, Tomoyo

AU - Sekino, Tohru

AU - Zarkov, Aleksej

PY - 2023/7/10

Y1 - 2023/7/10

N2 - Magnesium whitlockite (Mg-WH, Ca18Mg2(HPO4)2(PO4)12) is a promising candidate for biomedical application in bone regeneration; however, the fabrication of Mg-WH bioceramics by conventional methods is limited. Mg-WH is known to be thermally unstable and decomposes upon heating. The mechanism of thermal decomposition and phase evolution has not comprehensively been investigated so far. In the present work, Mg-WH was synthesized by a dissolution-precipitation process under hydrothermal conditions. Thermally induced degradation of the synthesized powders was investigated in detail by combining X-ray diffraction (XRD) analysis, infrared spectroscopy (FTIR), Raman spectroscopy as well as 1H and 31P solid-state nuclear magnetic resonance (NMR). The as-prepared Mg-WH powders were annealed at different temperatures in the range from 400 to 1300 °C. It was found that thermal decomposition starts at around 700 °C with the formation of beta-tricalcium phosphate (β-TCP, Ca3(PO4)2) and a mixture of two Ca2P2O7 polymorphs. Thermal decomposition occurs gradually and the co-existence of both Mg-WH and Mg-substituted β-TCP phases was observed in a wide temperature range up to 1200 °C. Complete disappearance of the HPO42− structural unit was confirmed only after annealing at 1300 °C followed by melting at 1400 °C.

AB - Magnesium whitlockite (Mg-WH, Ca18Mg2(HPO4)2(PO4)12) is a promising candidate for biomedical application in bone regeneration; however, the fabrication of Mg-WH bioceramics by conventional methods is limited. Mg-WH is known to be thermally unstable and decomposes upon heating. The mechanism of thermal decomposition and phase evolution has not comprehensively been investigated so far. In the present work, Mg-WH was synthesized by a dissolution-precipitation process under hydrothermal conditions. Thermally induced degradation of the synthesized powders was investigated in detail by combining X-ray diffraction (XRD) analysis, infrared spectroscopy (FTIR), Raman spectroscopy as well as 1H and 31P solid-state nuclear magnetic resonance (NMR). The as-prepared Mg-WH powders were annealed at different temperatures in the range from 400 to 1300 °C. It was found that thermal decomposition starts at around 700 °C with the formation of beta-tricalcium phosphate (β-TCP, Ca3(PO4)2) and a mixture of two Ca2P2O7 polymorphs. Thermal decomposition occurs gradually and the co-existence of both Mg-WH and Mg-substituted β-TCP phases was observed in a wide temperature range up to 1200 °C. Complete disappearance of the HPO42− structural unit was confirmed only after annealing at 1300 °C followed by melting at 1400 °C.

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Dissolution-precipitation synthesis and thermal stability of magnesium whitlockite

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