Probing the complex thermo-mechanical properties of a 3D-printed polylactide-hydroxyapatite composite using in situ synchrotron X-ray scattering

Polylactide (PLA)-hydroxyapatite (HAp) composite components have attracted extensive attentions for a variety of biomedical applications. This study seeks to explore how the biocompatible PLA matrix and the bioactive HAp fillers respond to thermo-mechanical environment of a PLA-HAp composite manufactured by 3D printing using Fused Filament Fabrication (FFF). The insight is obtained by in situ synchrotron small- and wide- angle X-ray scattering (SAXS/WAXS) techniques. The thermo-mechanical cyclic loading tests (0–20 MPa, 22–56 C) revealed strain softening (Mullins effect) of PLA-HAp composite at both room and elevated temperatures (50 C) due to the increased chain mobility. Above this temperature the deformation behaviour of the soft PLA lamella changes drastically. The thermal test (0–110 C) identified multiple crystallisation mechanisms of the PLA amorphous matrix, including reversible stressinduced large crystal formation at room temperature, reversible coupled stress-temperature-induced PLA crystal formation appearing at around 60 C, as well as irreversible heating-induced crystallisation above 92 C. The shape memory test (0– MPa, 0–70 C) of the PLA-HAp composite demonstrates a fixing ratio (strain upon unloading/strain before unloading) of 65% and rather a 100% recovery ratio, showing an improved shape memory property. These findings provide a new framework for systematic characterisation of the thermo-mechanical response of composites, and open up ways towards improved material design and enhanced functionality for biomedical applications. | Probing the complex thermo-mechanical properties of a 3D-printed polylactide-hydroxyapatite composite using in situ synchrotron X-ray scattering

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