Reactive Spreading of a Lead-Free Solder on Alumina

The wetting of Sn3Ag-based alloys on Al{sub 2}O{sub 3} has been studied using the sessile-drop configuration. Small additions of Ti decrease the contact angle of Sn3Ag alloys on alumina from 115 to 23 degrees. Adsorption of Ti-species at the solid-liquid interface prior to reaction is the driving force for the observed decrease in contact angle, and the spreading kinetics is controlled by the kinetics of Ti dissolution into the molten alloy. The addition of Ti increases the transport rates at the solid-liquid interface, resulting in the formation of triple-line ridges that pin the liquid front and promote a wide variability in the final contact angles

Effect of grain orientation and magnesium doping on β-tricalcium phosphate resorption behavior

The efficiency of calcium phosphate (CaP) bone substitutes can be improved by tuning their resorption rate. The influence of both crystal orientation and ion doping on resorption is here investigated for beta-tricalcium phosphate (β-TCP). Non-doped and Mg-doped (1 and 6 mol%) sintered β-TCP samples were immersed in acidic solution (pH 4.4) to mimic the environmental conditions found underneath active osteoclasts. The surfaces of β-TCP samples were observed after acid-etching and compared to surfaces after osteoclastic resorption assays. β-TCP grains exhibited similar patterns with characteristic intra-crystalline pillars after acid-etching and after cell-mediated resorption. Electron BackScatter Diffraction analyses, coupled with Scanning Electron Microscopy, Inductively Coupled Plasma–Mass Spectrometry and X-Ray Diffraction, demonstrated the influence of both grain orientation and doping on the process and kinetics of resorption. Grains with c-axis nearly perpendicular to the surface were preferentially etched in non-doped β-TCP samples, whereas all grains with simple axis (a, b or c) nearly normal to the surface were etched in 6 mol% Mg-doped samples. In addition, both the dissolution rate and the percentage of etched surface were lower in Mg-doped specimens. Finally, the alignment direction of the intra-crystalline pillars was correlated with the preferential direction for dissolution. Statement of significance: The present work focuses on the resorption behavior of calcium phosphate bioceramics. A simple and cost-effective alternative to osteoclast culture was implemented to identify which material features drive resorption. For the first time, it was demonstrated that crystal orientation, measured by Electron Backscatter Diffraction, is the discriminating factor between grains, which resorbed first, and grains, which resorbed slower. It also elucidated how resorption kinetics can be tuned by doping β-tricalcium phosphate with ions of interest. Doping with magnesium impacted lattice parameters. Therefore, the crystal orientations, which preferentially resorbed, changed, explaining the solubility decrease. These important findings pave the way for the design of optimized bone graft substitutes with tailored resorption kinetics

The in vitro evolution of resorbable brushite cements: A physico-chemical, micro-structural and mechanical study

The mechanisms by which calcium phosphate bone substitutes evolve and are resorbed in vivo are not yet fully known. In particular, the formation of intermediate phases during resorption and evolution of the mechanical properties may be of crucial interest for their clinical efficiency. The in vitro tests proposed here are the first steps toward understanding these phenomena. Microporous Dicalcium Phosphate Dihydrate (DCPD) samples were immersed in tris(hydroxymethyl)aminomethane (TRIS) and Phosphate Buffered Saline (PBS) solutions, with or without daily refresh of the medium, for time-points up to 14 days. Before and after immersion, samples were extensively characterised in terms of morphology, chemistry (XRD coupled with Rietveld analysis), microstructure (X-ray tomography, SEM observations) and local mechanical properties (instrumented micro-indentation). The composition of the immersion solutions was monitored in parallel (pH, elemental analysis). The results show the influence and importance of the experimental set-up and protocol on the formation of apatite and octacalcium phosphate concurrently to DCPD dissolution; moreover, strong inter-correlations between physico-chemistry, microstructure and mechanics are demonstrated. Statement of Significance Ideally, the resorption kinetics of biodegradable bone substitutes should be controlled to favor the healing processes of bone. Although biodegradable bone grafts are already used in surgeries, their resorption process is still partially unknown. The present work studies these resorption phenomena, their kinetics and mechanisms and their consequences on the properties of a calcium phosphate resorbable material. The original in vitro approach developed in this work couples for the first time physico-chemical, micro-structural and mechanical assessments. The dissolution of the CaP phase in body fluids and the reprecipitation of more stable phases are studied on a local scale, which has permitted to evidence and monitor the development of a gradient of properties between the surface and the core of the samples

Near-Infrared radiative properties of porous zirconia ceramics

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Sintering behavior of 45S5 Bioglass (R)

20th International Symposium on Ceramics in Medicine, Nantes, FRANCE, OCT 24-26, 2007International audienceIn this study, we report on the effect of Bioglass (R) structural transformations on its sintering behaviour. In a previous paper, we showed that while heating up to 1000 degrees C, five successive transformations Occur: glassy transition, phase separation, two crystallization processes and a second glassy transition. The sintering of the material exhibits two main shrinkage stages associated to the two glassy transitions at 550 degrees C and 850 degrees C. At 580 degrees C, the glass-in-glass phase separation induces a decrease of the sintering rate immediately followed by the crystallisation of the major phase Na2CaSi2O6 between 600 and 700 degrees C, from the surface to the bulk of the particles. A completed inhibition of sintering takes place followed by a minor shrinkage due to volume crystallization. A plateau is observed until the second glassy transition