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

Controlling calcium and phosphate ion release of 3D printed bioactive ceramic scaffolds: An in vitro study

his paper characterizes in an in vitro setting the release of calcium (Ca) and phosphate (PO4) of 3D printed bioactive ceramic scaffold prepared from extrudable paste containing hydroxyapatite and β-tricalcium phosphate (β-TCP). Hydroxyapatite and β-TCP were calcined at 800 °C for 11 h, fabricated into four experimental groups (100% HA, 100% β-TCP, 15%/85% HA/β-TCP, and 15%/85% HA/β-TCP (design)), sintered to 1100 °C for 4 h. Calcium and phosphorus concentrations were evaluated using ICP spectroscopy, and the release of Ca and PO4 ions during dissolution of the CaP-based scaffolds was measured by submerging in 0.05 mol/L Tris(hydroxymethyl)aminomethane-HCl and maintaining a temperature of 37 °C. The Ca and PO4 concentrations of the solutions were measured with the utilization of a calcium assay kit and a phosphate assay kit and read in a UV–visible spectrophotometer. The 100% HA scaffold group showed the greatest concentration of Ca ions (~1.9 mg/dL), but ultimately released at a lower amount as time increased; the 100% HA scaffold also showed the lowest total amount of calcium ions released over the course of evaluation. The results for the 100% β-TCP were on the opposite of the HA with the highest amount of calcium ion release over the study. While the PO4 ion release showed a similar trend as those observed with Ca ions with an apparent difference in the 100% HA scaffold group. There was nearly 0 mg/dL of the phosphate ions released in the first 24 h, in comparison to the amount of Ca ions released during the same time frame. Since various formulations can lead to different properties of these bioactive ceramic scaffolds, it is important to understand how the tailoring of this important biphasic material can impact the long-term outcome of an ever-important in vivo clinical trial in the future.Peer reviewedChemical Engineerin

Mg-substituted tricalcium phosphates: Formation and properties

This study aimed to investigate the formation and properties of magnesium (Mg)-substituted tricalcium phosphate, beta-TCMP, its properties and potential as biomaterial for bone repair. beta-TCMPs were prepared and characterized using x-ray diffraction, FT-IR and SEM. Dissolution properties were determined in acidic buffer. beta-TCMP discs were implanted in surgically created holes in femoral and tibial diaphyses of rabbits. Results demonstrated that the formation of beta-TCMP and Mg incorporation in beta-TCMP were dependent on reaction pH, temperature and solution Mg/Ca ratios. Sintered beta-TCMP was significantly less soluble than beta-TCP. Implanted unsintered beta-TCMP showed osteoconductive properties associated with new bone formation. This study suggests that beta-TCMP (sintered or unsintered), alone or in combination with other calcium phosphates, may be useful as biomaterials for bone repair and maybe useful in cases where slower biodegradation than that of beta-TCP is desire