Sintering effects on chemical and physical properties of bioactive ceramics

The objective of this study was to characterize the chemical and physical properties of bioactive ceramics prepared from an aqueous paste containing hydroxyapatite (HA) and beta tri-calcium phosphate (β-TCP). Prior to formulating the paste, HA and β-TCP were calcined at 800 °C and 975 °C (11 h), milled, and blended into 15%/85% HA/β-TCP volume-mixed paste. Fabricated cylindrical rods were subsequently sintered to 900 °C, 1100 °C or 1250 °C. The sintered specimens were characterized by helium pycnometry, X-ray diffraction (XRD), Fourier transform-infrared (FT-IR), and inductively coupled plasma (ICP) spectroscopy for evaluation of porosity, crystalline phase, functional-groups, and Ca:P ratio, respectively. Mechanical properties were assessed via 3-point bending and diametral compression. Qualitative microstructural evaluation using scanning electron microscopy (SEM) showed larger pores and a broader pore size distribution (PSD) for materials sintered at 900 °C and 1100 °C, whereas the 1250 °C samples showed more uniform PSD. Porosity quantification showed significantly higher porosity for materials sintered to 900 °C and 1250 °C (p< 0.05). XRD indicated substantial deviations from the 15%/85% HA/β-TCP formulation following sintering where lower amounts of HA were observed when sintering temperature was increased. Mechanical testing demonstrated significant differences between calcination temperatures and different sintering regimes (p < 0.05). Variation in chemical composition and mechanical properties of bioactive ceramics were direct consequences of calcination and sintering.Peer reviewedChemical Engineerin

Robocast Pb(Zr{sub 0.95}Ti{sub 0.05})O{sub 3} Ceramic Monoliths and Composites

Robocasting, a computer controlled slurry deposition technique, was used to fabricate ceramic monoliths and composites of chemically prepared Pb(Zr{sub 0.95}Ti{sub 0.05})O{sub 3} (PZT 95/5) ceramics. Densities and electrical properties of the robocast samples were equivalent to those obtained for cold isostatically pressed (CIP) parts formed at 200 MPa. Robocast composites consisting of alternate layers of the following sintered densities: (93.9%--96.1%--93.9%), were fabricated using different levels of organic pore former additions. Modification from a single to a multiple material deposition robocaster was essential to the fabrication of composites that could withstand repeated cycles of saturated polarization switching under 30 kV/cm fields. Further, these composites withstood 500 MPa hydrostatic pressure induced poled ferroelectric (FE) to antiferroelectric (AFE) phase transformation during which strain differences on the order of 0.8% occurred between composite elements

Properties of Polylactide Inks for Solvent-Cast Printing of Three-Dimensional Freeform Microstructures

ABSTRACT: Solvent-cast printing is a highly versatile microfabrication technique that can be used to construct various geometries such as filaments, towers, scaffolds and freeform circular spirals by the robotic deposition of a polymer solution ink onto a moving stage. In this work, we have performed a comprehensive characterization of the solvent-cast printing process using polylactide (PLA) solutions by analyzing the flow behavior of the solutions, the solvent evaporation kinetics and the effect of process-related parameters on the crystallization of the extruded filaments. Rotational rheometry at low to moderate shear rates showed a nearly Newtonian behavior of the PLA solutions, while capillary flow analysis based on process-related data indicated shear-thinning at high shear rates. Solvent vaporization tests suggested that the internal diffusion of the solvent through the filaments controlled the solvent removal of the extrudates. Different kinds of three-dimensional (3D) structures including a layer-by-layer tower, 9-layer scaffold and freeform spiral were fabricated, and a processing map was given to show the proper ranges of process-related parameters (i.e., polymer content, applied pressure, nozzle diameter and robot velocity) for the different geometries. The results of differential scanning calorimetry revealed that slow solvent evaporation could increase the ability of PLA to complete its crystallization process during the filament drying stage. The method developed here offers a new perspective for manufacturing complex structures from polymer solutions and provide guidelines to optimize the various parameters for 3D geometry fabrication