Preparation and Characterization of Multi-shell Hollow Biphase Bioceramic Microsphere Composites

doi:10.3724/SP.J.1077.2014.13501

Abstract

Abstract:

A series of hollow bioceramic microspheres with two or three shell layers were fabricated via alginate microsphere template and layer-by-layer coating techniques. The Na₂SiO₃-alginate mixture hydrosol beads were firstly injected into the Ca(NO₃)₂ aqueous solution under mild stirring to form calcium silicate hydrate-coated alginate microspheres. The composite microspheres were dispersed into the beta-tricalcium phosphate (β-TCP) -containing alginate hydrosol and wollastonite (CaSiO₃)-containing alginate hydrosol in turn while gently stirring. The microspheres were filtered, dried in vacuum and finally calcined at 850℃ for 2 h to obtain the multi-shell hollow bi-phase ceramic microspheres. The microstructure and chemical composition of the microspheres were characterized by SEM, EDX, XRD and FTIR analysis. In vitro biodegradation behavior of the two-shell hollow microspheres was tested in weak acidic Tris buffer and confirmed a unique controlled release characteristic for the silicate and phosphate groups. These results suggest that the rational design of the two- or multi-shell layer allows the preparation of bioceramic composites composed of β-TCP and CaSiO₃ with stage adjustable biodegradation and these biomaterials are potential candidates for improving bone regeneration and repair.

Key words: stage adjustable degradation, multi-shell hollow microspheres, wollastonate, β-TCP, bioceramics

CLC Number:

TQ174

YANG Yong-Zhu, ZHANG Lei, YANG Guo-Jing, GAO Chang-You, GOU Zhong-Ru. Preparation and Characterization of Multi-shell Hollow Biphase Bioceramic Microsphere Composites[J]. Journal of Inorganic Materials, 2014, 29(6): 650-656.

Figures/Tables 7

Fig. 1 Proposed multi-shell hollow microspheres preparation process and the superstructures of the ceramic microspheres

Fig. 2 Photographs of the microspheres before drying (a), after drying (b) and after calcination (c) and SEM images (d,e) of the superstructures of the single-shell CaSi microspheres

Fig. 3 Morphology before drying (a), microstructrue (b-d) and EDX spectra (e, f) of the two-shell CaSi@CaP hollow microspheres after calcination.

Fig. 4 Macromorphology before drying (a) and SEM images (b-f) of the three-shell CaSi@CaP@CaSi hollow microspheres showing the crosssection microstructures (b) and the three shell layers after calcination (c-f)

Fig. 5 XRD patterns of the as-calcined CaAlg microspheres (a), single-shell CaSi hollow microspheres (b), and two-shell CaSi@CaP hollow microspheres (c)

Fig. 6 FTIR spectra of the pure β-TCP (a), single-shell CaSi hollow microspheres (b) and two-shell CaSi@CaP hollow microspheres (c)

Fig. 7 Changes in Ca, P, and Si concentrations in the Tris buffer with initial pH 5.2 during soaking the two-shell CaSi@CaP (a) and CaP@CaSi (b) hollow ceramic microspheres

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