Effect of Al2TiO5 Content and Sintering Temperature on the Microstructure and Residual Stress of Al2O3-Al2TiO5 Ceramic Composites.

A series of Al2O3-Al2TiO5 ceramic composites with different Al2TiO5 contents (10 and 40 vol.%) fabricated at different sintering temperatures (1450 and 1550 °C) was studied in the present work. The microstructure, crystallite structure, and through-thickness residual stress of these composites were investigated by scanning electron microscopy, X-ray diffraction, time-of-flight neutron diffraction, and Rietveld analysis. Lattice parameter variations and individual peak shifts were analyzed to calculate the mean phase stresses in the Al2O3 matrix and Al2TiO5 particulates as well as the peak-specific residual stresses for different hkl reflections of each phase. The results showed that the microstructure of the composites was affected by the Al2TiO5 content and sintering temperature. Moreover, as the Al2TiO5 grain size increased, microcracking occurred, resulting in decreased flexure strength. The sintering temperatures at 1450 and 1550 °C ensured the complete formation of Al2TiO5 during the reaction sintering and the subsequent cooling of Al2O3-Al2TiO5 composites. Some decomposition of AT occurred at the sintering temperature of 1550 °C. The mean phase residual stresses in Al2TiO5 particulates are tensile, and those in the Al2O3 matrix are compressive, with virtually flat through-thickness residual stress profiles in bulk samples. Owing to the thermal expansion anisotropy in the individual phase, the sign and magnitude of peak-specific residual stress values highly depend on individual hkl reflection. Both mean phase and peak-specific residual stresses were found to be dependent on the Al2TiO5 content and sintering temperature of Al2O3-Al2TiO5 composites, since the different developed microstructures can produce stress-relief microcracks. The present work is beneficial for developing Al2O3-Al2TiO5 composites with controlled microstructure and residual stress, which are crucial for achieving the desired thermal and mechanical properties.

Mechanical properties of zirconia ceramics biomimetically coated with calcium deficient hydroxyapatite.

Mechanical properties and stability of porous tetragonal yttria-stabilised zirconia (Y-TZ) ceramics, biomimetically coated with calcium deficient hydroxyapatite (CaDHA) to obtain a bioactive material, were investigated. The 5.7 mol% yttria-stabilised tetragonal zirconia was obtained by sol-gel process and sintered at different temperatures to obtain a homogeneous and porous structure whose strength would match that of human bone. Sufficient strength was achieved by sintering at 1400 °C. The CaDHA coating was obtained at room temperature by a simplified preparation method consisting of immersion of the Y-TZ ceramics into a calcifying solution, after a short surface pretreatment in HCl. Although HAP or ß-TCP are more frequently used, CaDHA was chosen due to its structural similarity to the bone mineral and ability to support bone ingrowth to a greater extent than biphasic calcium phosphates. To verify the applicability CaDHA coatings, we tested their adherence to Y-TZ ceramics for the first time to the best of our knowledge. Vickers hardness (3.8 ± 0.2 GPa) reflected the hardness of underlying ceramic. The tensile strength (269 ± 52 MPa) and Weibull modulus (5) of the obtained biomaterials matched or exceeded those of bone. There was no statistical difference in the tensile strength between the coated (269 ± 52 MPa) and the uncoated (239 ± 46 MPa) ceramics. The Y-TZ-CaDHA coating system presented adequate structural integrity under scratch test with critical load for coating cracking of 18 ± 2 N. These results indicate the potential of the prepared bioceramic to be used as bone implants.

Diopside-tricalcium phosphate bioactive ceramics for osteogenic differentiation of human adipose stem cells.

Ti scaffolds combined with autologous human adipose-derived mesenchymal stem cells (hASCs) have been successfully applied for regenerative cranio-maxillofacial bone therapies. Future challenges reside in regeneration of larger bone defects and displacement of the permanent Ti structure, thus, advanced resorbable scaffolds are needed. Composites of ß-Ca3 (PO4 )2 with 80 and 60 wt % of CaMg(SiO3 )2 with improved mechanical properties compared to tricalcium phosphate (TCP) materials are presented. Synthetic CaMg(SiO3 )2 and a precursor of Ca3 (PO4 )2 were used to fabricate the composites and a reference ß-Ca3 (PO4 )2 material by uniaxial pressing and solid state sintering. Optimum sintering temperature of 1225°C was selected. Microstructural analysis and Weibull distributions of tensile strengths determined by the diametral compression of discs test are reported. Thermodynamic simulation of the dissolution process in simulated body fluid body fluid was done. The biological response with hASCs was analyzed using basic and osteogenic media. Viability and osteogenic potential-LIVE/DEAD assay; alkaline phosphatase activity and collagen type-I production-were characterized. The composites have higher tensile strength (>3×) than TCP materials, for similar reliability, and support viability and osteogenic differentiation of hASCs. Resorption of the high strength phase diopside is the slowest. The promising results reported here suggest possible uses of these bioactive ß-Ca3 (PO4 )2 -CaMg(SiO3 )2 ceramics together with hASCs in bone tissue engineering.

Effect of graphene on setting and mechanical behaviour of tricalcium phosphate bioactive cements.

The potential reinforcing effect of graphene on calcium phosphate cements (CPCs) for injectable bone substitutes and scaffolds is presented. The influence of graphene (0-3.84 vol%) on the microstructural development during setting and the resultant mechanical properties of CPCs constituted by α + ß-tricalcium phosphate is analysed. Optimum setting conditions were established using uniaxial compression strength of CPC and composites with pristine and functionalized graphene and liquid/solid ratios (L/S = 0.5-0.6 mL/g) that allowed the mixing and spatulation of the powders. Tensile strength of optimised materials has been determined using the Diametric Compression of Discs Test (DCDT). X-ray diffraction, Raman spectroscopy and FE-SEM-EDS on fracture surfaces were used to investigate phase composition and morphological changes in set specimens. Strengthening occurs for functionalized graphene additions up to 1.96 vol% due to different toughening mechanisms. Crack deflection, bridging and branching by graphene and, finally, the pull-out of the unbroken graphene sheets have been identified. Interlayer sliding between the graphene before pulling-out is an additional toughening process. Main effect of graphene on strength is the increase of reliability.

In vitro study of the proliferation and growth of human fetal osteoblasts on Mg and Si co-substituted tricalcium phosphate ceramics.

The objective of this work was to study the feasibility of the solid state sintering, a conventional ceramic processing method, to obtain Mg and Si co-substituted tricalcium phosphate bioceramics and composites containing diopside. A series of new Ca3 (PO4 )2 based ceramics has been prepared from attrition milled mixtures of synthetic Ca3 (PO4 )2 and CaMg(SiO3 )2 powders, isostatically pressed and sintered at 1250-1300°C. Materials containing 0, 1, and 5 wt % of CaMg(SiO3 )2 were constituted by ß + α - Ca3 (PO4 )2 solid solutions while the material containing 60 wt % of CaMg(SiO3 )2 was a constituted by ß- Ca3 (PO4 )2 and CaMg(SiO3 )2 . The biological responses of the developed ceramics were studied in vitro using human fetal osteoblast cultures. Culture times ranged from 1 to 21 days. The new family of materials promotes the adhesion and proliferation of human osteoblasts cultured onto their surface forming a monolayer and showing a normal morphology. The results of the MTT and Alamar Blue assays showed that the soluble components extracted from the Mg/Si- co-substituted Ca3 (PO4 )2 and the Ca3 (PO4 )2 -CaMg(SiO3 )2 composite were noncytotoxic. The specimens with diopside exhibited a better in vitro behavior which is attributed to the release of Si and Mg ions to the culture medium, enhancing the activity of cells. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 105A: 2266-2275, 2017.

Bone neoformation of a novel porous resorbable Si-Ca-P-based ceramic with osteoconductive properties: physical and mechanical characterization, histological and histomorphometric study.

OBJECTIVE: The aims of the present work were to study a new porous Nurse's A ceramic (Si-Ca-P-based material) bone substitute and examine its mechanical properties in vitro and the biocompatibility, osteoconductivity and resorption process in vivo. MATERIALS AND METHOD: Porous ceramic scaffolds were prepared by solid-state reaction and implanted in critical-sized defect created in 15 NZ rabbits. Strength values were determined by the diametrical compression of disk test. Weibull analyses were performed following the European Standard for technical ceramics EN-843-5: 1996, considering 90% of confidence intervals. Results were correlated with scanning microscope observations of fracture surfaces. Implanted scaffolds were characterized by histological and histomorphometric point of view. RESULTS: The parameters of the Weibull distribution of strength, determined by diametrical compression of disks, were modulus m = 13, and characteristic strength σ0  = 0.60 MPa (90% confidence limit: m = 7.2-17.6, σ0  = 0.570-0.578). Porous calcium silicophosphate scaffolds showed significantly more bone formation in the pores and in the periphery of the implant than the control group. Histomorphometric analysis revealed that the ceramic scaffold (62.23 ± 0.34*) produced higher values of bone-to-implant contact (BIC) percentages (higher quality, closer contact); moreover, defect closure was significative in relation with control group. CONCLUSIONS: The porous calcium silicophosphate ceramic is biocompatible, partially resorbable and osteoinductive material. This rabbit study provides radiological and histological evidences confirming the suitablity of this new material for bone tissue regeneration on critical defects.

Effect of Mg and Si co-substitution on microstructure and strength of tricalcium phosphate ceramics.

Magnesium and silicon co-doped tricalcium phosphate (TCP) ceramics with compositions corresponding to 0, 5 and 10wt% CaMg(SiO3)2 in the system Ca3(PO4)2-CaMg(SiO3)2 were obtained by conventional sintering of compacted mixtures of Ca3(PO4)2, MgO, SiO2 and CaCO3 powders at temperatures between 1100 and 1450°C. Microstructural analyses were performed by X-ray diffraction and field emission scanning electron microscopy with energy dispersive spectroscopy. Major phases in the obtained ceramics were ß- or α+ß-tricalcium phosphate containing Mg and Si in solid solution. Certain amounts of liquid were formed during sintering depending on composition and temperature. There were found significant differences in distributions of strength determined by the diametral compression of disc tests (DCDT). Failure strengths were controlled by microstructural defects associated with phase development. Mg and Si additions were found to be effective to improve densification and associated strength of TCP bioceramics due to the enhancement of sintering by the low viscosity liquids formed. The highest density and strength were obtained for the TCP ceramic containing 5wt% CaMg(SiO3)2 sintered at 1300°C. Cracking and porosity increased at higher temperatures due to grain growth and swelling.

Work of fracture of a composite resin: fracture-toughening mechanisms.

The aim of this work was to investigate those mechanical parameters able to describe the fracture behavior of dental composite resins. A commercially available fine-particle micro-hybrid resin composite was used. Classical parameters as Young's modulus, strength distribution, and critical stress intensity factor were considered. Strength values were determined using the diametrical compression of discs test and for the critical stress intensity factor both unstable and controlled fracture tests were used. Controlled fracture tests allowed determining the work of fracture. Microstructure was studied by optical and field emission scanning electron microscopy. The obtained properties have been Young's modulus, 17.7 +/- 0.6 GPa; Weibull modulus, m = 14 (upper and lower limits for 90% confidence: 17 and 10); characteristic strength 51 MPa (upper and lower limits for 90% confidence: 53 and 49 MPa); critical stress intensity factor in mode I, K(IC) = 1.3 +/- 0.1 and work of fracture, gamma(wof) = 8-9 J/m(2). Pores and bubbles formed during the packing of the composite were identified as critical defects in the tested specimens. Crack deflection and branching have been identified as toughening mechanisms. Classical mechanical parameters (Young's modulus, hardness...) are not able to efficiently predict the major clinical failure mode of composite resins by fatigue. Work of fracture analysis, which is dependant on microstructural parameters such as particle size and shape, have to be included when testing mechanical properties of dental composite resins in future research studies.