resumo
The Taguchi experimental design method is an elegant and efficient way of deriving optimum conditions for processes from the minimum number of experiments. We correlated various relevant synthesis parameters in the precipitation synthesis of single-phase pure hydroxyapatite (Ca-10(PO4)(6)(OH)(2), HAp) nanoparticles, via a rapid wet precipitation method, without any aging time. Taguchi planning was used for a systematic study of the combined effects of five different parameters: pH, synthesis temperature, synthesis time, drying temperature and calcination temperature. Using T\aguchi methods, we were able to evaluate the effects of four variations (levels) in each of these five parameters, with just 16 experiments (an L-16 (1024) orthogonal array). We assessed the impact of these parameters on four distinct properties, namely crystallite size, surface area, Ca/P atomic ratio and mol% of HAp. Calcination temperature exerted the greatest impact on hydroxyapatite morphology, corresponding to crystallite size and specific surface area, for which the role of other processing parameters was not significant. On the contrary, the Ca:P ratio was affected mainly by pH. These findings were confirmed by microstructural, structural and spectroscopic characterisation. FTIR spectra, revealing the conditions to retain a pure or prevailing hydroxyapatite phase, and also to indicate favourable conditions for A-type substitutions of carbonate for hydroxide groups, or B-type substitution for phosphate groups. (C) 2016 Elsevier Ltd. All rights reserved.
palavras-chave
SOL-GEL METHOD; CALCIUM HYDROXYAPATITE; NANOPARTICLES; POWDERS; PRECIPITATION; TEMPERATURE; MORPHOLOGY; PH
categoria
Materials Science
autores
Ben-Arfa, BAE; Salvado, IMM; Frade, JR; Pullar, RC
nossos autores
Basam Abobaker Emhmed Ben-Arfa
Investigador
Isabel Margarida Miranda Salvado
Professor associado
Jorge Ribeiro Frade
Professor(a) Jubilado(a)
Rob Pullar
ColaboradorGrupos
G3 - Materiais Eletroquímicos, Interfaces e Revestimentos
G4 - Materiais Renováveis e Economia Circular
G5 - Materiais Biomiméticos, Biológicos e Vivos
agradecimentos
R.C. Pullar was supported by FCT Grant SFRH/BPD/97115/2013 for this work. This work was developed in the scope of the project CICECO-Aveiro Institute of Materials (Ref. FCT UID/CTM/50011/2013), financed by national funds through the FCT/MEC and when applicable co-financed by FEDER under the PT2020 Partnership Agreement.