In-situ hydroxyapatite mineralization in beech and pine wood: effects of leaching on fire behavior

This study presents the in-situ synthesis of hydroxyapatite (HAp) within the structure of beech and pine wood. The modification process utilized a two-step vacuum-pressure impregnation coupled with chemical precipitation using calcium nitrate tetrahydrate and diammonium hydrogen phosphate solutions, followed by exposure to ammonium hydroxide vapors. While the initial focus was on the overall physicochemical changes, microstructural characteristics and fire behavior of the mineralized wood, the main aim is to specifically investigate the effects of leaching. Because HAp synthesis produces water-soluble ammonium nitrate (NH 4 NO 3 ) as a by-product, this research systematically addresses how the removal of this component affects the final properties of wood. HAp formation was confirmed by FTIR and X-ray diffraction, while scanning electron microscopy and microcomputed tomography revealed HAp deposits primarily in the cell lumen of both wood species. Fire behavior was evaluated using thermal analysis and the cone calorimeter. The incorporation of non-flammable HAp synthesized within the wood structure may act as a barrier and mass transfer during pyrolysis. This results to comparable or slightly enhanced key fire performance parameters when comparing leached HAp synthesized samples with leached reference samples. In contrast, the unleached HAp synthesized samples, which still contained residual NH 4 NO 3 , showed deterioration in fire growth rate (FIGRA) and heat release rate (HRR) parameters, confirming that NH 4 NO 3 acts as an oxidant. However, this oxidative property also leads to improvements in total heat release (THR) and total smoke production (TSP) parameters compared to unleached references, representing a complex interaction when studying the fire properties of mineralized wood.