Comprehensive structural studies of ultra-fine nanocrystalline calcium hydroxyapatite using MAS NMR and FT-IR spectroscopic methods

• Published in: Materials research bulletin 2013-11, Vol.48 (11), p.4818-4825
• Main Authors: Pajchel, Lukasz, Kowalska, Violetta, Smolen, Dariusz, Kedzierska, Aleksandra, Pietrzykowska, Elzbieta, Lojkowski, Witold, Kolodziejski, Waclaw
• Format: Article
• Language: English
• Subjects: A. Inorganic compounds; A. Nanostructures; A. Surfaces; Biological; C. Infrared spectroscopy; C. Nuclear magnetic resonance (NMR); Crystals; Infrared spectroscopy; Nanocomposites; Nanomaterials; Nanostructure; Nuclear magnetic resonance; Reaction time
• ISSN: 0025-5408; 1873-4227
• DOI: 10.1016/j.materresbull.2013.08.048

•We studied three nanoapatites (HAP) prepared by microwave solvothermal synthesis.•We used NMR and FT-IR to characterize ultra-fine HAP particles.•The HAP particles had crystal core, hydrated layer and external liquid-like zone.•We determined various physicochemical characteristics of those discrete regions.•We found substantial deficiency and disorder of structural hydroxyl ions. Three nanoapatites produced using a microwave solvothermal synthesis (MSS), including one with a mean crystal size of only 6nm, were characterized by high-resolution solid-state NMR (1H and 31P) and FT-IR spectroscopies. It was found that nanoapatite particles had an inner crystal core covered by a non-apatitic surface hydrated layer with an outermost liquid-like zone. Various physicochemical properties of those apatite compartments were determined. Important structural details, such as deficiency and disorder of structural OH− ions were discovered and discussed. The materials were also compared with respect to the reaction time and thermal post-synthesis treatment in order to optimize their preparation conditions to the required performance. The study emphasizes the influence of the surface hydrated layer on the physicochemical properties and biological activity of nanoapatites.