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Micro-extrusion-based 3D printing of complex geometrical and porous calcium phosphate (CaP) can improve treatment of bone defects through the production of personalized bone substitutes. However, achieving printing and post-printing shape stabilities for the efficient fabrication and application of rapid hardening protocol are still challenging. In this work, the coaxial printing of a self-setting CaP cement with water and ethanol mixtures aiming to increase the ink yield stress upon extrusion and the stability of fabricated structures was explored. Printing height of overhang structure was doubled when aqueous solvents were used and a 2 log increase of the stiffness was achieved post-printing. A standard and fast steam sterilization protocol applied as hardening step on the coaxial printed CaP cement (CPC) ink resulted in constructs with 4 to 5 times higher compressive moduli in comparison to extrusion process in the absence of solvent. This improved mechanical performance is likely due to rapid CPC setting, preventing cracks formation during hardening process. Thus, coaxial micro-extrusion-based 3D printing of a CPC ink with aqueous solvent enhances printability and allows the use of the widespread steam sterilization cycle as a standalone post-processing technique for production of 3D printed personalized CaP bone substitutes. Statement of significance Coaxial micro-extrusion-based 3D printing of a self-setting CaP cement with water:ethanol mixtures increased the ink yield stress upon extrusion and the stability of fabricated structures. Printing height of overhang structure was doubled when aqueous solvents were used, and a 2 orders of magnitude log increase of the stiffness was achieved post-printing. A fast hardening step consisting of a standard steam sterilization was applied. Four to 5 times higher compressive moduli was obtained for hardened coaxially printed constructs. This improved mechanical performance is likely due to rapid CPC setting in the coaxial printing, preventing cracks formation during hardening process.

3Y-TZP discs were coated using 5Y-PSZ and 12Ce-TZP suspensions. Samples were evaluated in terms of roughness (Ra, Rq, Rz and Rsk), B3B flexural resistance, hardness, Young's modulus by instrumented indentation and surface damage resistance and Vickers hardness by impress Vickers measurements. Coatings with thickness of ~7 μm were obtained. 3Y-TZP uncoated discs showed similar hardness and Young's modulus when compared to those coated with 5Y-PSZ. Discs coated with 12Ce-TZP had opposite behavior. Vickers and Berkovich hardness showed the same trend, with almost no difference observed between monolithic and the 5Y-PSZ coated samples, and with the 12Ce-TZP coated samples exhibiting lower hardness values. Coated samples presented lower flexural strength than uncoated ones. Correlation between roughness and B3B flexural strength was also performed, showing that surface quality achieved by the coating process is the one that rules the final resistance of the component, instead of the coating material.

Objectives The presentin vitro study evaluated the effect of LTD (Low Temperature Degradation) on microstructural properties, phase transformation and micro-crack formation of 5 commercially and non-commercially available Zirconia dental implant systems. Methods Accelerated ageing at 134 °C and 2 bar pressure for 30 h was completed. Focused Ion Beam-Scanning Electron Microscopy (FIB/SEM), X-ray diffraction (XRD) and cathodoluminescence quantified phase transformation and micro-crack formation. Results Transformation of the tetragonal grains towards the monoclinic symmetry was observed in all systems. The highest depth was measured in non-commercial TAV dental with the largest grain size (8.7 μm). A micro-cracked layer was associated with the transformation zone. The ageing-related micro-crack formation was parallel to the surface for all groups and was deepest for the non-commercial TAV dental with the largest grain size (7.4 μm). Conclusion LTD following in vitro ageing using an autoclave was minimal for all implant systems investigated.

To develop durable bone healing strategies through improved control of bone repair, it is of critical importance to understand the mechanisms of bone mechanical integrity when in contact with biomaterials and implants. Bone mechanical integrity is defined here as the adaptation of structural properties of remodeled bone in regard to an applied mechanical loading. Accordingly, the authors present why future investigations in bone repair and regeneration should emphasize osteocytes that surround matrices. Osteocytes are mechanosensitive cells considered as the orchestrators of bone remodeling, which is the biological process involved in bone homeostasis. These bone cells are trapped in an interconnected porous network, the lacunocanalicular network, which is embedded in a bone mineralized extracellular matrix. As a consequence of an applied mechanical loading, the bone deformation results in the deformation of this lacunocanalicular network inducing a shift in interstitial fluid pressure and velocity, thus resulting in osteocyte stimulation. The material environment surrounding each osteocyte, the so called perilacunar and pericellular matrices properties, define its mechanosensitivity. While this mechanical stimulation pathway is well known, the laws used to predict bone remodeling are based on strains developing at a tissue scale, suggesting that these strains are related to the shift in fluid pressure and velocity at the lacunocanalicular scale. While this relationship has been validated through observation in healthy bone, the fluid behavior at the bone-implant interface is more complex. The presence of the implant modifies fluid behavior, so that for the same strain at a tissue scale, the shift in fluid pressure and velocity will be different than in a healthy bone tissue. In that context, new markers for bone mechanical integrity, considering fluid behavior, have to be defined. The viewpoint exposed by the authors indicates that the properties of the pericellular and the perilacunar matrices have to be systematically investigated and used as structural markers of fluid behavior in the course of bone biomaterial development.

International audience; Objective. Healing of soft tissues and improvement of aesthetics have become major research objectives in implantology and renewed the interest for ceramics implants. The aim of this study was to evaluate the pre-clinical performance of screw-shaped sandblasted-etched implants processed from an innovative zirconia-based ceramic composite, in comparison to titanium. Methods. Twenty-four ceramic and twenty-four titanium screw-shaped sandblasted-etched dental implants were tested in a splitmouth design in six Beagle dogs. Surface topographies were investigated by confocal microscopy. Local tissue effects were evaluated at 4 and 13 weeks after implantation through histology. An ANOVA statistical analysis (5% risk; p

Poly(l-lactide-co-d,l-lactide) PDLA/45S5 Bioglass® (BG) composites for medical devices were developed using an original approach based on a thermal treatment of BG prior to processing. The aim of the present work is to gain a fundamental understanding of the relationships between the morphology, processing conditions and final properties of these biomaterials. A rheological study was performed to evaluate and model the PDLA/BG degradation during processing. The filler contents, as well as their thermal treatments, were investigated. The degradation of PDLA was also investigated by Fourier transform infrared (FTIR) spectroscopy, size-exclusion chromatography (SEC) and mechanical characterization. The results highlight the value of thermally treating the BG in order to control the degradation of the polymer during the process. The present work provides a guideline for obtaining composites with a well-controlled particle dispersion, optimized mechanical properties and limited degradation of the PDLA matrix.

Long-term, reliable operation of Solid Oxide fuel and electrolysis Cell (SOCs) necessitates cells with high strength and resistance to mechanical degradation. In this work, strength, Young’s modulus and Low-Temperature Degradation (LTD) of several zirconia-based SOCs supports are studied. The study shows that replacing 3YSZ with a tetragonal zirconia compound having lower stabilizer contents can improve the strength of porous supports. An enhancement up to 30 % over the-state-of-the-art support (NiO‒3YSZ) can be achieved for example with using NiO‒2.5YSZ. It is further evidenced that tetragonal zirconia-based SOC components (both Y-doped and Ce-Y co-doped) are susceptible to LTD in the studied range of grain sizes (i.e. ≈ 200−300 nm). Addition of small amount of alumina (0.5 wt%) is observed to increase the LTD resistance of porous supports. The susceptibility to LTD must be considered in designing materials for SOCs, also during materials processing, storage, handling and operation where a dry atmosphere is recommended.

The market share of zirconia (ZrO2) dental implants is steadily increasing. This material comprises a polymorphous character with three temperature-dependent crystalline structures, namely monoclinic (m), tetragonal (t) and cubic (c) phases. Special attention is given to the tetragonal phase when maintained in a metastable state at room temperature. Metastable tetragonal grains allow for the beneficial phenomenon of Phase Transformation Toughening (PTT), resulting in a high fracture resistance, but may lead to an undesired surface transformation to the monoclinic phase in a humid environment (low-temperature degradation, LTD, often referred to as ‘ageing’). Today, the clinical safety of zirconia dental implants by means of long-term stability is being addressed by two international ISO standards. These standards impose different experimental setups concerning the dynamic fatigue resistance of the final product (ISO 14801) or the ageing behavior of a standardized sample (ISO 13356) separately. However, when evaluating zirconia dental implants pre-clinically, oral environmental conditions should be simulated to the extent possible by combining a hydrothermal treatment and dynamic fatigue. For failure analysis, phase transformation might be quantified by non-destructive techniques, such as X-Ray Diffraction (XRD) or Raman spectroscopy, whereas Scanning Electron Microscopy (SEM) of cross-sections or Focused Ion Beam (FIB) sections might be used for visualization of the monoclinic layer growth in depth. Finally, a minimum load should be defined for static loading to fracture. The purpose of this communication is to contribute to the current discussion on how to optimize the aforementioned standards in order to guarantee clinical safety for the patients.

International audience; Ceramic-on-ceramic bearings in total hip replacement have shown the potential to provide low wear solutions in hip replacement. Assessing the tribological performance of these materials is important to predict their long-term performance in patients. In this study, a methodology was devised to assess the tribological in vitro behaviour of composite ceramics under combined adverse edge loading conditions and accelerated ageing. Two commercial ceramic composites were considered, namely Alumina-Toughened Zirconia (ATZ, ceramys®) and Zirconia-Toughened Alumina (ZTA, symarec®). The bearing couples were studied using the Leeds Mark II hip joint simulator for a total of eight million cycles, the first two million under normal gait (no edge loading) and the following six million cycles with the addition of edge loading conditions driven by medial-lateral separation. The bearing couples underwent hydrothermal ageing using an accelerated protocol in autoclave every million cycles. The influence of edge loading combined with ageing was significant for ATZ bearings, resulting in a slower overall ageing kinetics over the wear stripe than on the control heads. During the autoclave ageing steps, the monoclinic fraction increased more over the wear stripe area than over the unworn area. Both results thus indicated that the monoclinic phase was removed during shocks induced by edge loading. The wear performance of the two materials were similar exhibiting relatively low wear rates and low level of microstructural damage for these clinically relevant adverse conditions.

International audience; Osteomalacia is a pathological bone condition consisting in adeficient primary mineralization of the matrix, leading to an accumulation of osteoid tissue and reduced bone mechanical strength. The amounts, properties and organization of bone constituents at tissue level, are known to influence its mechanical properties. It is then important to investigate the relationship between mechanical behavior and tissue composition at this scale in order to provide a better understanding of bone fragility mechanisms associates with this pathology. Our purpose was to analyze the links between ultra-structural properties and the mechanical behavior of this pathological bone tissue (osteomalacia) at tissue level (mineral and osteoidseparately, or global). Four bone biopsies were taken from patients with osteomalacia, and subsequently embedded, sectioned, and polished.Then nanoindentation tests were performed to determine local elastic modulus E, contact hardness Hc and true hardness H for both mineralized and organic bone phases and for the global bone. The creep of the bone was also studied using a special indentation procedure in order to assess visco-elasto-plastic (creep) bone behavior. This allowed a detailed study of the rheological models adapted to the bone and to calculate the parameters associated to a Burgers model. Ultra-structural parameters were measured by Fourier Transform InfraRed Microspectroscopy (FTIRM) on the same position as the indents.The use of rheological models confirmed a significant contribution from the organic phase on the viscous character of bone tissue. The elastic E and the elasto-plastic Hc deformation were correlated to both collagen maturity and Mineral/Matrix. The pure plastic deformation H was only correlated to the mineral phase. Our data show that mineral phase greatly affects mechanical variables (moduli and viscosities) and that organic phase (as illustrated in osteoidtissue) may play an important role in the creep behavior of bone.In conclusion, this study brings mechanical and physicochemical values for osteoid and mineral phases

Transformation-induced plasticity in a ceria-stabilized-zirconia based composite was studied in four-point bending, with particular emphasis on nucleation and growth of tetragonal-to-monoclinic transformation bands. They initiated on the side in tension at a given value of stress and grow in size and number with increased applied load. The spacing between them was related to samples’ thickness: thicker samples led to a smaller number of larger/deeper bands. Residual stresses around indentations, placed on the tensile surface of some samples, triggered transformation bands nucleation but had no significant effect on the final total number of bands. A simple stress shielding model suggests that wide bands hinder adjacent thinner bands to propagate and expand because of stress shielding around them. Nucleation of a given transformation band is thus related to: (i) stress concentrations at the surface, (ii) geometry (stress-field inside the sample) and (iii) a shielding effect from the bands already present.

International audience; Two-photon lithography is a potential route to produce high-resolution 3D ceramics. However, the large shrinkage due to the elimination of an impor-tant organic counterpart of the printed material during debinding/sintering remains a lock to further development of this technology. To limit this phenomenon, an original approach based on a composite resin incorporating 45 wt% ultrasmall (5 nm) zirconia stabilized nanoparticles into the zirconium acrylate precursor is proposed to process 3D zirconia microlattices and nano-structured optical surfaces. Interestingly, the nanoparticles are used both as seeds allowing control of the crystallographic phase formed during the calcination process and as structural stabilizing agent preventing important shrinkage of the printed ceramic. After 3D photolithography and pyrolysis, the weight and volume loss of the microstructures are drastically reduced as compared to similar systems processed with the reference resin without nanoparticles, and stable 3D microstructures of cubic zirconia are obtained with high spatial resolution. In the case of a patterned surface, the refractive index of 2.1 leads to a diffraction efficiency large enough to obtain microfo-cusing with linewidths of 0.1 μm, and the demonstration of a microlens array with a period as small as 0.8 μm

Magnesium oxide nanocubes are compressed along the [001] direction in situ in the transmission electron microscope. Incipient plasticity in the smaller samples is characterized by the nucleation of few $ \raise.5ex\hbox{$\scriptstyle 1$}\kern-.1em/\kern-.15em\lower.25ex\hbox{$\scriptstyle 2$} {\lt}110{\gt} \{{110} \} $ dislocations while a larger number of line defects is observed in larger nanocubes. Yield and flow stresses scattered stochastically above a minimum value varying as the inverse of the sample size. The upper bound is given by the reduced number of dislocation sources. Such size-dependent behaviour is justified by a detailed statistical analysis and is fully explained by the deformation mechanism.

International audience; Meso-porous γ-alumina ceramics used as catalyst supports are characterized by high porosity fraction (>70%) and specific surface area (>200 m²/g) targeted to ensure high catalytic performances, but at the expense of the mechanical strength. The aim of this work is to link the mechanical properties of three different catalyst supports with their microstructure. Instrumented indentation tests were performed at two different length scales to assess mechanical properties at both macroscopic scale (support) and at constituents scale (grains and matrices). The distribution of porosity fraction in grains and matrices is estimated with image processing on Scanning Electron Microscopy (SEM) pictures. The mechanical behavior of catalyst supports are strongly influenced by their microstructure. In spite of a larger porosity fraction, macro-and meso-porous grains exhibit higher mechanical properties than the matrices. Matrix of the three alumina supports have almost similar volume fraction of porosity but different mechanical properties. Finally, Focused Ion Beam (FIB) cross-sections of residual indents indicate a damageable behavior under contact loading, with densification of larger pores.

International audience; Thin, porous zirconia-based ceramic components are of high interest in energy application devices where they are used as structural ceramics. Mechanical reliability of such devices is not only dependent on the fracture toughness of the ceramic components, but also on their sensitivity to slow crack growth (SCG). In this work, the fracture toughness and SCG behavior of porous (4.5 to 45.5%) and thin (~ 0.25 mm) 3Y-TZP ceramics are investigated using the Double Torsion method. The analysis of the double torsion data, previously developed for dense materials, was here assessed and adapted. The compliance of the samples was observed to change linearly with crack length and the measured stress intensity factor was dependent on crack length, as for dense materials. This dependency decreased by increasing the sample porosity. For all materials, the ratio of the SCG threshold to fracture toughness was of 0.56 ± 0.06.

International audience; Individual platelets in nacre‐like ceramics are able to locally withstand stress levels many times larger than the strength of larger specimens made of the same materials. This size effect, usually reported as being relative to the size of pre‐existing defects, is described by considering both stress and energy failure conditions. We show that there is a characteristic length, defined by the material's Young's modulus, fracture energy, and strength, above which failure is governed by a stress criterion and below which energy considerations are dominant. Applying the coupled criterion to three‐point bending of a single alumina platelet allows the identification of the platelet strength and fracture energy. The proposed approach also allows capturing the decrease in failure stress due to a surface defect accounting for its shape and size.

In this work, the effect of substituting Cu with small amounts of Sn and Si on the passive behavior and pitting resistance of the bulk metallic glass Ti40Zr10Cu36Pd14 was investigated. The Sn/Si substitution promoted homogenization of the solid solution and limited the presence of casting defects. In addition, unlike the heterogeneous passive film grown on TiZrCuPd, the passive films of the micro-alloyed materials were homogeneous, implying less sensitivity to film weakening and breakdown. Thus, alloying with small amounts of Sn and Si appears to be a viable approach to drastically improve the corrosion resistance of TiZrCuPd.

Further development and upscaling of the Solid Oxide fuel and electrolysis Cell (SOCs) technologies would significantly benefit from improvement of their mechanical robustness. In this work, microstructure, crystalline phase composition, fracture toughness and susceptibility to low- and high-temperature degradation of six different Ni(O)‒Zirconia fuel electrode supports, manufactured from six different stabilized zirconia compounds, are investigated. In the oxidized state, tetragonal zirconia-based supports have higher fracture toughness than cubic zirconia-based substrate, due to the transformation toughening effect and a finer grained microstructure. The NiO‒1.5CeO2 4.5YO1.5-SZ support exhibits the highest fracture toughness, showing a 30 and 10 % improvement compared to the state-of-the-art NiO‒5.8YO1.5-SZ support at room temperature and 800 °C, respectively. In the reduced state on the other hand, the tetragonal and cubic zirconia-based substrates have comparable fracture toughness. The Ceria-Yttria co-doped materials possess superior resistance to hydrothermal degradation due to the stabilizing effect of Ce3+ formed during reduction.

OBJECTIVES: To evaluate two-body wear of three zirconia ceramics stabilized with 3, 4 and 5mol% yttria and to compare their wear behavior with that of a lithium-disilicate glass-ceramic. METHODS: Sixteen rectangular-shaped specimens made from three grades of zirconia ceramics and a lithium-disilicate glass-ceramic were polished and dynamically loaded in a chewing simulator (2kg vertical load, 2.1Hz) under water at 90°C for 1.2×106 cycles (about 7 days) in the ball-on-plate mode against steatite antagonists. Surface roughness was measured before and after wear testing. Wear tracks were scanned with a non-contact 3D profilometer and super-impositions were used to determine wear loss of the antagonists. Wear surfaces were imaged by SEM. XRD and micro-Raman spectroscopy were used to characterize phase transformation and stress status in the worn and unworn areas of the zirconia ceramics. RESULTS: Independent of fracture toughness, strength and aging-susceptibility, the three zirconia ceramics showed a similar and limited amount of wear (∼10μm in depth) and were more wear-resistant than the lithium-disilicate glass-ceramic (∼880μm in depth). Abrasive wear without obvious cracks was observed for all investigated zirconias, whereas the glass-ceramic with a lower fatigue threshold and high susceptibility to surface dissolution exhibited significant abrasion, fatigue and corrosion wear. All three zirconia ceramics yielded a lower antagonist wear than the glass-ceramic and no significant differences were found between the zirconia ceramics. SIGNIFICANCE: In the context of this study, high-translucent zirconia ceramics stabilized with a higher yttria content, recently introduced in the dental field, were as wear-resistant and antagonist-friendly as conventional high-strength zirconia and suitable for monolithic restorations. ispartof: DENTAL MATERIALS vol:35 issue:12 pages:1776-1790 ispartof: location:England status: published

International audience; 40 years ago, Garvie and his Australian co-workers reported that the stress induced transformation of metastable tetragonal zirconia grains to the monoclinic symmetry could give rise to a powerful toughening mechanism. Their results even led them to consider zirconia systems as analogues of certain steels. This seminal paper generated extraordinary excitement in the ceramic community and it is still the subject of extensive research. Transformation toughening is widely used in zirconia materials and results in an increase in strength and toughness when compared to non-transformable ceramics, but the implementation into strong, tough, and sufficiently stable materials has not been fully reached. Zirconia ceramics generally fail at low strains with a much larger scatter in the strength values than metals and require statistical approaches to failure. Here we describe in details the mechanical behavior laws of ceria-doped zirconia composites exhibiting a high degree of stress-induced transformation. They present, to some extent, mechanical behavior analogous to a metal, displaying, i) significant amount of transformation-induced plasticity without damage, ii) very high flaw

cited By 0; International audience; Twenty-year-old samples of (Mg,Y)-PSZ—Spinel composite were characterized to assess their microstructure and mechanical properties after such a long period of natural aging. The amount of the different phases was determined by XRD, whereas a detailed observation of the microstructural features was carried out by high-resolution SEM and FIB/SEM. Bending strength, hardness, and toughness were also measured. Translucency was quantified by measuring the contrast ratio (CR). After comparison of the results obtained in this study with those obtained 20 years ago, the studied material reveals a phase stability superior to that exhibited by conventional 3Y-TZP, good strength, and hardness and a remarkable toughness. The value of CR is comparable with those exhibited by the materials commonly used in dentistry. Thanks to the presence of spinel particles, grains are smaller than in conventional Mg-PSZ. In addition, we show here that grains can be further refined through spark plasma sntering. For all these reasons (Mg,Y)-PSZ-spinel composite could be proposed as valid alternative to 3Y-TZP for dental applications. © 2018 The American Ceramic Society

International audience; Hydrothermal ageing is one lifetime-limiting phenomenon of zirconia-based ceramics and composites for many applications, from biomedical implants to ferrules and watches. Predicting hydrothermal ageing at use-temperature implies a set of accelerated ageing experiments conducted under water vapour at several, high temperatures (usually between 100°C and 140°C). From these data, the activation energy of ageing can be determined, and thus ageing can be predicted at any temperature. However, obtaining precise extrapolations with this procedure requires the use of lower temperatures (70 or 80°C), leading to a rather long procedure (up to a few thousand hours), and should involve at least one specimen for each test temperature. This article presents a new procedure that allows the determination of all ageing parameters and the estimation of kinetics at use-temperatures with the use of a single specimen within a shorter time, accurate enough for fast screening of new materials.

International audience; Recent studies on zirconia-toughened alumina (ZTA) evidenced that in vivo aged implants display a much higher monoclinic zirconia content than expected from in vitro simulations by autoclaving. At the moment, there is no agreement on the source of this discrepancy: Some research groups ascribe it to the effect of mechanical impact shocks, which are generally not implemented in standard in vitro aging or hip walking simulators. Others invoke the effect of metal transfer, which should trigger an autocatalytic reaction in the body fluid environment, accelerating the kinetics of tetragonal-to-monoclinic transformation in vivo. Extrapolations of the aging kinetics from high (autoclave) to in vivo temperature are also often disputed. Last, Raman spectroscopy is by far the preferred method to quantify the amount of monoclinically transformed zirconia. There are, however, many sources of errors that may negatively affect Raman results, meaning that the final interpretation might be flawed. In this work, we applied Raman spectroscopy to determine the monoclinic content in as-received and in vitro aged ZTA hip joint implants, and in one long-term retrieval study. We calculated the monoclinic content with the most used equations in the literature and compared it with the results of X-ray diffraction obtained on a similar probe depth. Our results show, contrary to many previous studies, that the long-term surface stability of ZTA ceramics is preserved. This suggests that the Raman technique does not offer consistent and unique results for the analysis of surface degradation. Moreover, we discuss here that tetragonal-to-monoclinic transformation is also necessary to limit contact damage and wear stripe extension. Thus, the surface metastability of zirconia-containing ceramics may be a non-issue.

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.

X-ray Computed Tomography (XCT) analysis was applied to identify and quantify typical defects in dense 3Y-TZP zirconia processed by the Lithography-based Ceramic Manufacturing (LCM) technique. XCT derived strengths were anticipated from the XCT data and compared to experimental measurement. A good agreement between XCT data, bending strength measurement and fractographic analysis demonstrates the suitability of X-ray tomography for both defects detection and predictive mechanical strength estimation. It allows also to rank the different defects related to LCM in terms of their criticality versus mechanical resistance.

cited By 2; International audience; Scaffolds for bone tissue engineering require a combination of bioactivity and bioresorption at the sample surface and high mechanical properties in the bulk. This work presents a novel calcium phosphate (CaP)/polycaprolactone (PCL) scaffold with graded composition and porosity fraction. The scaffold is made of (i) a dense hydroxyapatite (HA)/β-tricalcium phosphate (β-TCP) core, (ii) a macroporous HA/β-TCP transition layer and (iii) a macroporous PCL/(HA/β-TCP) external layer. The ceramic layers were fabricated by gel-casting whereas the outer composite layer was obtained by a solvent casting/particle leaching process. The microstructure, phase composition and biodegradation of the scaffolds were characterized. The gradient of porosity was clearly obtained whereas the gradation of phase composition was less pronounced. An in vitro dissolution test was performed by immersing the scaffolds in a TRIS solution. The results showed a dissolution phenomenon with possible differentiated mechanisms in the different layers, in relation with the targeted multi-functionality. © 2018 Elsevier B.V.

© 2018 Elsevier Ltd Slow crack growth (SCG) behavior of four zirconia-based composites reinforced with 40 vol% WC, TiC, NbC or TiCN were studied by means of double-torsion testing. Compared to monolithic zirconia, the composites had a higher resistance to fast fracture, i.e., higher fracture toughness. The extent of toughening depended on the reinforcement type, shifting the V-KI (crack velocity versus stress intensity factor) curve parallel to higher KI values. More importantly, these composites were less sensitive to SCG. Identical V-KI/KIC curves with steeper slopes compared to monolithic zirconia were observed for the investigated composites, independent on the reinforcement type. No rising R-curve was measured, at least in the crack-size domain investigated by SCG. Therefore, the higher SCG resistance of the composites was due to the intrinsic stress-assisted corrosion resistance of the covalent non-oxide secondary phase. ispartof: JOURNAL OF THE EUROPEAN CERAMIC SOCIETY vol:39 issue:2-3 pages:641-646 status: published

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 objective of this paper is to review the current knowledge on the development of nanostructured zirconia-based ceramics and composites suitable for application in dentistry. Isi Web of Science, Science Direct, Scientific.net databases, and Google were searched electronically for the period of 1980 to the present, matching the keywords “nano” with the keywords: “Zirconia, ZrO2, Y-TZP, and dental, dentistry”. A total of 74 papers were found, with the majority coming from Asia, indicating a more active scientific interest on the topic in this geographic area, followed by Europe, South America, and North America. The research shows, even though the scientific activity on nanostructured ceramics was intense in the last fifteen years, the development of fully dense zirconia-based nanoceramics is yet at an initial stage, most of all from the point of view of the clinical applications. It has been demonstrated that nanostructured ceramics can show improved properties because of the reduction of the grain size to the nanoscale. This is also true for zirconia-based nanoceramics, where some improvements in mechanical, optical, as well as resistance in low-temperature degradation have been observed. Potential applications of this class of material in the dental field are discussed, summarizing the results of the latest scientific research.

cited By 0; Resorbable ceramics used as porous bone substitutes are designed to favor bone in-growth and to be gradually replaced by natural tissues after in vivo resorption. However, a lack of experimental techniques to quantitatively monitor the evolution of their mechanical properties during resorption is noted. In this paper, we propose to use spherical instrumented indentation to follow-up the resorption of microporous resorbable ceramics at a local scale. Tests were performed at the core and at the surface of samples immersed for different durations in model fluids. Instrumented indentation was found to be an efficient technique to characterize and to follow-up the resorption of microporous ceramics, in excellent agreement with microstructural changes observed with X-ray diffraction and X-ray tomography. Instrumented indentation has the ability to capture the presence of gradients in the samples, enables the direct testing of wet samples and appears as a superior technique to compression tests mostly used in the literature. © 2019 Elsevier Ltd

High strength and translucency are generally not coincident in one restorative material and there is still a continuous development for a better balance between these two properties. Zirconia and lithium-disilicate glass-ceramics are currently the most popular alternatives for monolithic restorations. In this work, the mechanical properties and more important, the slow crack growth (SCG) resistance, which rules long-term durability, were thoroughly studied for three zirconia ceramics stabilized by 3, 4 and 5 mol% yttria in comparison to lithium-disilicate glass-ceramic. Translucency versus strength maps revealed that the more translucent zirconia compositions (i.e. with higher yttria contents) fill the gap between the standard 3 mol% yttria stabilized zirconia (3Y-TZP) and lithium-disilicate. Moreover, increasing yttria content did not always result in lower strength, as values for 3 mol% and 4 mol% yttria were the same. Independent on the yttria contents, all zirconia showed similar relative susceptibility to SCG under static and cyclic conditions and were significantly more SCG-resistant than lithium-disilicate glass ceramic. A concern with higher yttria contents (5 and 4 mol%) however could lie in the higher sensitivity to defects, resulting in a larger scatter in strength. STATEMENT OF SIGNIFICANCE: In addition to the common investigations on the generally reported strength, toughness and translucency, V-KI diagrams (crack velocity versus stress-intensity factor) from fast fracture to threshold for three newly developed zirconia were directly measured by double torsion methods under static and cyclic loading conditions. The crack-growth mechanisms were analyzed in depth. Results were compared with another popular dental ceramic, namely lithium-disilicate glass-ceramic, revealing the pros and cons of polycrystalline and glass-ceramics in terms of long-term durability. This is the first time that V-KI curves are compared for the major ceramic and glass-ceramic used for dental restorations. Strength versus translucency maps for different CAD/CAM dental restorative materials were described, showing the current indication range for zirconia ceramics. ispartof: ACTA BIOMATERIALIA vol:91 pages:24-34 ispartof: location:England status: published

International audience; This paper aims at identifying the multiaxial compression behavior of highly porous ceramics used ascatalyst supports. For this purpose, instrumented spherical indentation tests are performed, togetherwith uniaxial and hydrostatic compression tests. A transition from a brittle to a damageable behaviorwith densification of the material is noted when increasing the triaxiality of the test. The collapse of largepores is shown as being responsible for the densification phenomenon, as confirmed by SEM andmercury intrusion porosimetry. A multiaxial damage criterion is proposed and identified thanks to anumerical finite element model.The results described in this paper coupled with a previous work (Staub et al., Oil and gas science andtechnology 2015, vol 70, n 3, 475e86) on the behavior of the same material under tension loading, allowfor the first time to define a multiaxial criterion both in tension and in compression for highly porousceramics. These materials are shown to present a typical behavior of dense ceramics in tension, whereasin compression, their behavior is close to that of porous rocks.

The aging behavior of 3-mol%-yttria-stabilized tetragonal zirconia (3Y-TZP) ceramics sintered in air and in reducing conditions was investigated at 140{\deg}C in water vapor. It was observed by X-ray diffraction (XRD) that 3Y-TZP samples sintered in reducing conditions exhibited significantly higher tetragonal-to-monoclinic transformation than samples with similar density and average grain size values but obtained by sintering in air. This fact is explained by the increase of the oxygen vacancy concentration and by the presence at the grain boundary region of a new aggregate phase formed because of the exolution of Fe2+ ions observed by X-ray photoelectron spectroscopy., Comment: 10 pages, 3 figures

International audience; Literature is quite abundant concerning the resorption of calcium phosphates. However, articles on in vitro acellular dissolution tests are scarcer, although these immersion experiments are often considered a first step in establishing a predictive dissolution test and understanding the resorption mechanisms. Also, the comparison of results obtained after immersion in model fluids reveals large discrepancies.The first part of this paper is a literature review focused on in vitro aging of apatite, dicalcium phosphate dihydrate (DCPD) and beta tricalcium phosphate (β-TCP). In the second part, experimental findings obtained by immersing DCPD and β-TCP samples in TRIS and PBS solutions for different times demonstrate the influence of the immersion conditions and possible artefacts induced by the experimental protocols. Suggestions are provided to improve the design of in vitro experiments. In addition, the interest to follow-up at the same time and at a local scale physico-chemical, microstructural and mechanical properties is discussed.