Continuous-flow precipitation of hydroxyapatite in ultrasonic microsystems

• Published in: Chemical engineering journal (Lausanne, Switzerland : 1996) Vol. 215-216; no. 15; pp. 979 - 987
• Main Authors: Castro, Filipa, Kuhn, Simon, Jensen, Klavs, Ferreira, António, Rocha, Fernando, Vicente, António, Teixeira, José António
• Format: Journal Article
• Language: English
• Published: Elsevier B.V 2013
• Subjects: Aggregation; aqueous solutions; chemical engineering; crystal structure; Hydroxyapatite; Microfluidics; Nanoparticles; particle size; temperature; ultrasonics; Ultrasound; Nanoparticles; Aggregation; Hydroxyapatite; Ultrasound; Microfluidics
• ISSN: 1385-8947; 1873-3212
• DOI: 10.1016/j.cej.2012.11.014

► Continuous-flow precipitation of HAp was studied in two ultrasonic microreactors. ► A tubular reactor and a novel Teflon reactor were investigated. ► Laminar flow and segmented flow were both evaluated. ► Both reactors produce HAp under near-physiological conditions of temperature and pH. ► HAp particles with improved properties were obtained in a short time. This paper describes the continuous-flow precipitation of hydroxyapatite Ca5(PO4)3OH (HAp) in two ultrasonic microreactors using diluted aqueous solutions of calcium and phosphate at 37°C. Precipitation of HAp was first carried out in a tubular microreactor immersed in an ultrasonic bath, where single-phase (laminar) flow and segmented gas–liquid flow were both evaluated. The single-phase flow study was then conducted in a novel microfluidic device developed at MIT. It consists of a Teflon stack microreactor with an integrated piezoelectric element (Teflon microreactor), thereby allowing the direct transmission of ultrasound to the reactor. Both microsystems produce single-phased calcium-deficient carbonated HAp under near-physiological conditions of temperature and pH. In addition, particle aggregation and primary particle size were significantly reduced in the segmented-flow tubular microreactor and in the Teflon microreactor. The as-prepared particles mostly consisted of rod-like shape nanoparticles with dimensions below 100nm in length and around 20nm in width. Further, the microreactors used yielded HAp particles with improved characteristics, namely higher crystallinity and less carbonate contamination, when compared to the HAp particles produced in a stirred tank batch reactor.