Maria Angeles Cattani-Lorente

Low temperature degradation of a Y-TZP dental ceramic

Bars of Y-TZP ceramic for dental restorations were subjected to hydrothermal degradation via in vitro exposure to water steam at 140°C for 7 days. X-ray diffraction, atomic force microscopy and scanning electron microscopy techniques were applied to observe and quantify the tetragonal-monoclinic (t-m) phase transformation associated with the process. Nanoindentation was used to assess the ceramics mechanical properties before and after hydrothermal degradation. Texture associated with martensitic t-m transformation was observed at the grain surface. The t-m transformation followed nucleation-and-growth kinetics, with predominance of the nucleation process. The transformation occurred within a layer of 6 μm below the surface. Mechanical properties deteriorated with hydrothermal degradation, resulting in a 30% reduction of Youngs modulus and hardness. A strong correlation was found between the increasing monoclinic fraction and the decline in mechanical response. It was thus concluded that the emergence of the monoclinic phase and the associated microcracking were the most likely causes for the degradation of mechanical properties.

Comparative study of the physical properties of a polyacid-modified composite resin and a resin-modified glass ionomer cement

OBJECTIVES The physical properties of the resin-modified composite resin Dyract (Detrey Dentsply) and the resin-modified glass ionomer cement Fuji II LC (GC) were compared, and the effect of water sorption on these properties was studied. METHODS Compressive, diametral compressive and flexural strengths were measured using specimens aged up to three months. The Vickers hardness and the water erosion were also determined. The specimens were stored at 37 degrees C under five different conditions, chosen to vary the water sorption of the samples. The results were analyzed using a multi-factor analysis of variance. RESULTS Dry specimens of Dyract and Fuji II LC showed similar properties. However, the two materials behaved differently when stored in presence of water. In contrast to Fuji II LC, Dyract showed very little expansion for the first 24 h (1.5 +/- 0.3 and 0.03 +/- 0.01%, respectively), leached small quantities of ions and retained its mechanical strength. Those differences are related to their chemical composition. Fuji II LC is hydrophilic, as it contains polyHEMA. In the presence of water, Fuji II LC behaves like a hydrogel, but the network resulting from the copolymerization of acidic and UDMA monomers is less hydrophilic, and the effect of water on Dyract is retarded. SIGNIFICANCE The significant properties of Dyract are determined by its composite character. This certainly represents some advantages, for instance, a higher mechanical strength, a better protection against initial dehydration and subsequent water effects. However, Dyract shows some disadvantages over Fuji II LC, like a lower amount of fluoride release or the interference of oxygen during polymerization.

Early strength of glass ionomer cements

The present study compared the compressive, tensile and flexural strengths of 26 commercial glass ionomer cements, which were evaluated 24 h after the beginning of the setting reaction. In order to give a global estimation of their overall strength, a coefficient was attributed to each glass ionomer cement. This strength coefficient provided a ranking of the tested materials. The highest scores were obtained by the restorative glass ionomers; however, these materials exhibited lower mechanical properties than the more classic restorative materials such as amalgams or composites. The results also showed a large scattering of the mechanical properties among the luting and lining glass ionomer cements. The creep behavior of the glass ionomer cements was also investigated.

A new testing protocol for zirconia dental implants

OBJECTIVES Based on the current lack of standards concerning zirconia dental implants, we aim at developing a protocol to validate their functionality and safety prior their clinical use. The protocol is designed to account for the specific brittle nature of ceramics and the specific behavior of zirconia in terms of phase transformation. METHODS Several types of zirconia dental implants with different surface textures (porous, alveolar, rough) were assessed. The implants were first characterized in their as-received state by Scanning Electron Microscopy (SEM), Focused Ion Beam (FIB), X-Ray Diffraction (XRD). Fracture tests following a method adapted from ISO 14801 were conducted to evaluate their initial mechanical properties. Accelerated aging was performed on the implants, and XRD monoclinic content measured directly at their surface instead of using polished samples as in ISO 13356. The implants were then characterized again after aging. RESULTS Implants with an alveolar surface presented large defects. The protocol shows that such defects compromise the long-term mechanical properties. Implants with a porous surface exhibited sufficient strength but a significant sensitivity to aging. Even if associated to micro cracking clearly observed by FIB, aging did not decrease mechanical strength of the implants. SIGNIFICANCE As each dental implant company has its own process, all zirconia implants may behave differently, even if the starting powder is the same. Especially, surface modifications have a large influence on strength and aging resistance, which is not taken into account by the current standards. Protocols adapted from this work could be useful.

Hydrothermal degradation of a 3Y-TZP translucent dental ceramic: A comparison of numerical predictions with experimental data after 2 years of aging

OBJECTIVES The purpose of the study was to assess the hydrothermal resistance of a translucent zirconia with two clinical relevant surface textures by means of accelerated tests (LTD) and to compare predicted monoclinic fractions with experimental values measured after two years aging at 37°C. METHODS Polished (P) and ground (G) specimens were subjected to hydrothermal degradation by exposure to water steam at different temperatures and pressures. The t-m phase transformation was quantified by grazing incidence X-ray diffraction (GIXDR). The elastic modulus and hardness before- and after LTD were determined by nanoindentation. RESULTS G specimens presented a better resistance to hydrothermal degradation than P samples. Activation energies of 89 and 98kJ/mol and b coefficients of 2.0×10(-5) and 1.8×10(-6) were calculated for P and G samples respectively. The coefficients were subsequently used to predict transformed monoclinic fractions at 37°C. A good correlation was found between the predicted values and the experimental data obtained after aging at 37°C during 2 years. Hydrothermal degradation led to a significant decrease of the elastic moduli and hardness in both groups. SIGNIFICANCE The dependency of the t-m phase transformation rate on temperature must be determined to accurately predict the hydrothermal behavior of the zirconia ceramics at oral temperatures. The current prevailing assumption, that 5h aging at 134°C corresponds to 15-20 years at 37°C, will underestimate the transformed fraction of the translucent ceramic at 37°C. In this case, the mechanical surface treatment influences the ceramics transformability. While mild grinding could potentially retard the hydrothermal transformation, polishing after occlusal adjustment is recommended to prevent wear of the antagonist teeth and maintain structural strength.

Effect of different surface treatments on the hydrothermal degradation of a 3Y-TZP ceramic for dental implants

OBJECTIVES Implant surface modifications are intended to enhance bone integration. The objective of this study was to assess the effect of different surface treatments on the resistance to hydrothermal degradation, hardness and elastic modulus of a 3Y-TZP ceramic used for dental implants. METHODS Samples grouped according to their surface morphologies (AS, as-sintered; C, coated; P, dry-polished; R, roughened; PA, polished and annealed; RA, roughened and annealed) were subjected to accelerated hydrothermal degradation (LTD) by exposure to water steam (134°C, 2bars) for 100h. The t-m phase transformation was quantified by grazing incidence X-ray diffraction (GIXDR) and by combined focused ion beam and scanning electron microscopy (FIB-SEM). Elastic modulus and hardness before- and after prolonged aging (100h) were assessed by nanoindentation. RESULTS AS and C specimens presented a better resistance to hydrothermal degradation than P and R samples. After prolonged aging, the depth of the monoclinic transformed layer ranged from 11μm to 14μm. Hydrothermal degradation led to a significant decrease of elastic modulus and hardness. SIGNIFICANCE Surface treatments affected the resistance to hydrothermal degradation of the 3Y-TZP ceramic. Dry mechanical surface modifications should be avoided since a high t-m transformation rate associated to the initial monoclinic content was observed. Annealing was useful to reverse the initial t-m transformation, but did not improve the resistance to hydrothermal degradation.

TiNOx coatings on roughened titanium and CoCr alloy accelerate early osseointegration of dental implants in minipigs

INTRODUCTION Titanium nitride oxide (TiNOx) coatings are known for their biocompatibility, hardness and high resistance to corrosion and wear. Further, they can be applied by plasma vapor deposition onto a wide variety of metallic, mineral, or organic substrates. In cell cultures, TiNOx coatings applied onto SLA (sandblasted, large grit, acid etched)-roughened titanium surfaces increased human primary osteoblast proliferation by 1.5 times in the first 2 weeks after seeding, while maintaining a high degree of cell differentiation. Therefore, the objectives of the present study were (i) to determine whether these findings would translate into the enhanced osseointegration of TiNOx-coated implants in vivo and (ii) to compare the osseointegration of Ti-SLA (titanium-SLA) and CoCr-SLA (cobalt-chromium-SLA) implants coated with TiNOx. METHODS Forty-eight cylinders made of Ti-SLA, Ti-SLA-TiNOx (TiNOx-coated Ti-SLA) and CoCr-SLA-TiNOx (TiNOx-coated CoCr-SLA) were implanted into the lower jawbone of 8 minipigs. The bone-to-implant contact was determined after 1 week, 2 weeks, 1 month and 3 months. RESULTS Osseointegration proceeded normally on all 3 surfaces, with equal activity after the first week of healing. After 2 weeks, bone-to-implant contact was 1.8 times higher on TiNOx coatings, either deposited on Ti or on CoCr. These differences fell off after 1 and 3 months of healing. CONCLUSIONS When compared to standard SLA titanium, TiNOx coatings enhance implant osseointegration during the first month of healing. Furthermore, this stimulating effect is independent of the substrate, leading to similar results whether the coating is applied onto SLA-Ti or onto SLA-CoCr.

Grinding damage assessment for CAD-CAM restorative materials

OBJECTIVES To assess surface/subsurface damage after grinding with diamond discs on five CAD-CAM restorative materials and to estimate potential losses in strength based on crack size measurements of the generated damage. METHODS The materials tested were: Lithium disilicate (LIT) glass-ceramic (e.max CAD), leucite glass-ceramic (LEU) (Empress CAD), feldspar ceramic (VM2) (Vita Mark II), feldspar ceramic-resin infiltrated (EN) (Enamic) and a composite reinforced with nano ceramics (LU) (Lava Ultimate). Specimens were cut from CAD-CAM blocs and pair-wise mirror polished for the bonded interface technique. Top surfaces were ground with diamond discs of respectively 75, 54 and 18μm. Chip damage was measured on the bonded interface using SEM. Fracture mechanics relationships were used to estimate fracture stresses based on average and maximum chip depths assuming these to represent strength limiting flaws subjected to tension and to calculate potential losses in strength compared to manufacturers data. RESULTS Grinding with a 75μm diamond disc induced on a bonded interface critical chips averaging 100μm with a potential strength loss estimated between 33% and 54% for all three glass-ceramics (LIT, LEU, VM2). The softer materials EN and LU were little damage susceptible with chips averaging respectively 26μm and 17μm with no loss in strength. Grinding with 18μm diamond discs was still quite detrimental for LIT with average chip sizes of 43μm and a potential strength loss of 42%. SIGNIFICANCE It is essential to understand that when grinding glass-ceramics or feldspar ceramics with diamond discs surface and subsurface damage are induced which have the potential of lowering the strength of the ceramic. Careful polishing steps should be carried out after grinding especially when dealing with glass-ceramics.

Grinding damage assessment on four high-strength ceramics

OBJECTIVES The purpose of this study was to assess surface and subsurface damage on 4 CAD-CAM high-strength ceramics after grinding with diamond disks of 75 μm, 54 μm and 18 μm and to estimate strength losses based on damage crack sizes. METHODS The materials tested were: 3Y-TZP (Lava), dense Al2O3 (In-Ceram AL), alumina glass-infiltrated (In-Ceram ALUMINA) and alumina-zirconia glass-infiltrated (In-Ceram ZIRCONIA). Rectangular specimens with 2 mirror polished orthogonal sides were bonded pairwise together prior to degrading the top polished surface with diamond disks of either 75 μm, 54 μm or 18 μm. The induced chip damage was evaluated on the bonded interface using SEM for chip depth measurements. Fracture mechanics were used to estimate fracture stresses based on average and maximum chip depths considering these as critical flaws subjected to tension and to calculate possible losses in strength compared to manufacturers data. RESULTS 3Y-TZP was hardly affected by grinding chip damage viewed on the bonded interface. Average chip depths were of 12.7±5.2 μm when grinding with 75 μm diamond inducing an estimated loss of 12% in strength compared to manufacturers reported flexural strength values of 1100 MPa. Dense alumina showed elongated chip cracks and was suffering damage of an average chip depth of 48.2±16.3 μm after 75 μm grinding, representing an estimated loss in strength of 49%. Grinding with 54 μm was creating chips of 32.2±9.1 μm in average, representing a loss in strength of 23%. Alumina glass-infiltrated ceramic was exposed to chipping after 75 μm (mean chip size=62.4±19.3 μm) and 54 μm grinding (mean chip size=42.8±16.6 μm), with respectively 38% and 25% estimated loss in strength. Alumina-zirconia glass-infiltrated ceramic was mainly affected by 75 μm grinding damage with a chip average size of 56.8±15.1 μm, representing an estimated loss in strength of 34%. All four ceramics were not exposed to critical chipping at 18 μm diamond grinding. CONCLUSIONS Reshaping a ceramic framework post sintering should be avoided with final diamond grits of 75 μm as a general rule. For alumina and the glass-infiltrated alumina, using a 54 μm diamond still induces chip damage which may affect strength. Removal of such damage from a reshaped framework is mandatory by using sequentially finer diamonds prior to the application of veneering ceramics especially in critical areas such as margins, connectors and inner surfaces.

In vitro bone exposure to strontium improves bone material level properties

In rats treated with strontium ranelate, the ultimate load of intact bone is increased and associated with changes in microstructure and material level properties. Evaluation by micro-computed-tomography-based finite element analysis has shown that these changes independently contribute to the improvement of bone strength induced by strontium ranelate treatment. However, the mechanism by which Sr ion acts on bone material level properties remains unknown. The vertebrae of intact female rats were exposed overnight to 0.5, 1 or 2M chloride salt solutions of Sr, Ca and Ba. The latter two were used to assess the specificity of Sr. Bone material level properties were evaluated by measuring hardness, elastic modulus and working energy in a nanoindentation test. Wavelength dispersive X-ray spectroscopy provided semi-quantitative elemental analysis and mapping. Incubation with Sr rendered bone stiffer, harder and tougher. Among the divalent ions tested, Sr had the greatest effect. Sr affinity was also assessed on in vivo treated bone specimens. After in vitro exposure, the highest improvements were observed in ovariectomized rats. However, anti-osteoporotic treatments did not influence the capacity of Sr to modify bone material level properties. Our findings demonstrated that in vitro incubation with Sr selectively improved bone material level properties, which may contribute to the macroscopic increase of bone properties observed under Sr therapy.