Binary SiO2-CaO bioactive glass nanoparticles synthesis and colloidal stability investigated via in-situ SAXS for freeze-cast scaffolds
Abstract
Binary SiO 2 -CaO bioactive glass nanoparticles (NPs) are synthesized as the elementary bricks of freeze-cast (FC) macroscopic scaffolds envisioned for human mandible bone transplants. In-situ X-ray scattering at ultra-small, small and wide angles (USAXS/SAXS/WAXS) was used to monitor the successive steps involved in the production of the NPs and their stability in suspensions prior to FC. Time-resolved scattering (TR-SAXS) revealed the growth mechanisms of nanosilicate cores in aqueous solutions. Quantitative analysis in absolute scale of the intensity demonstrates that subsequent calcium incorporation strongly modifies the colloidal interactions via the formation of hydrated Ca²⁺/NO₃⁻ interfacial layers, that promote partial mass-fractal aggregation from reduced electrostatic repulsion. Upon transfer to organic FC solvents such as dimethyl carbonate, further ion condensation favors tenuous rod-like aggregation even for pure silica NPs. SAXS analysis combined with analytical centrifugation indicate that aggregation controls the homogeneity of the FC suspensions by greatly accelerating sedimentation, which can be mitigated by addition of free PDLLA chains. Operando phase-contrast X-ray computed tomography prior to FC further reveals the spatial NPs and aggregates distribution, that strongly influence the properties of the final scaffold network. This comprehensive multiscale framework linking nanoparticle synthesis and interactions, colloidal stability and FC suspensions homogeneity, provides new insights for the rational design of freeze-cast nanocomposite scaffolds.
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BibTeX
@article{pierron2026binary,
title = {{Binary SiO2-CaO bioactive glass nanoparticles synthesis and colloidal stability investigated via in-situ SAXS for freeze-cast scaffolds}},
author = {Alexandra Pierron and Isabelle Morfin and Prescillia Lagarrigue and Ludovic Broche and William Chèvremont and Thomas Bizien and Vincent Darcos and Jérémy Soulié and Guillaume Brotons},
journal = {Colloids and Surfaces A: Physicochemical and Engineering Aspects},
year = {2026},
month = nov,
doi = {10.1016/j.colsurfa.2026.141005},
url = {https://hal.science/hal-05854713v1},
note = {CC BY},
}
RIS
TY - JOUR
TI - Binary SiO2-CaO bioactive glass nanoparticles synthesis and colloidal stability investigated via in-situ SAXS for freeze-cast scaffolds
AU - Alexandra Pierron
AU - Isabelle Morfin
AU - Prescillia Lagarrigue
AU - Ludovic Broche
AU - William Chèvremont
AU - Thomas Bizien
AU - Vincent Darcos
AU - Jérémy Soulié
AU - Guillaume Brotons
PY - 2026
DA - 2026/11/06
JO - Colloids and Surfaces A: Physicochemical and Engineering Aspects
DO - 10.1016/j.colsurfa.2026.141005
UR - https://hal.science/hal-05854713v1
AB - Binary SiO 2 -CaO bioactive glass nanoparticles (NPs) are synthesized as the elementary bricks of freeze-cast (FC) macroscopic scaffolds envisioned for human mandible bone transplants. In-situ X-ray scattering at ultra-small, small and wide angles (USAXS/SAXS/WAXS) was used to monitor the successive steps involved in the production of the NPs and their stability in suspensions prior to FC. Time-resolved scattering (TR-SAXS) revealed the growth mechanisms of nanosilicate cores in aqueous solutions. Quantitative analysis in absolute scale of the intensity demonstrates that subsequent calcium incorporation strongly modifies the colloidal interactions via the formation of hydrated Ca²⁺/NO₃⁻ interfacial layers, that promote partial mass-fractal aggregation from reduced electrostatic repulsion. Upon transfer to organic FC solvents such as dimethyl carbonate, further ion condensation favors tenuous rod-like aggregation even for pure silica NPs. SAXS analysis combined with analytical centrifugation indicate that aggregation controls the homogeneity of the FC suspensions by greatly accelerating sedimentation, which can be mitigated by addition of free PDLLA chains. Operando phase-contrast X-ray computed tomography prior to FC further reveals the spatial NPs and aggregates distribution, that strongly influence the properties of the final scaffold network. This comprehensive multiscale framework linking nanoparticle synthesis and interactions, colloidal stability and FC suspensions homogeneity, provides new insights for the rational design of freeze-cast nanocomposite scaffolds.
SN - 0927-7757
SN - 1873-4359
ER -