Evaluation of bond strength between zirconia milled ceramic material and veneered dental porcelain.

This study aimed at examining the bond strength between zirconia and ceramic veneer, following the ISO 9693 guidelines. A total of fifty specimens of zirconia/ceramic-veneer system were produced using two commercial zirconias (VITA YZ-HTWhite and Zolid HT+ White, referred to as Group A and Group B, respectively) and a ceramic-veneering material (Zirkonia 750). The microstructure (via x-ray diffraction analysis, XRD and Secondary Electron mode, SEM) and the mechanical properties (via 3-point bending tests) of the two groups were assessed. Then, experiments were conducted according to the ISO 9693 and conventional protocols applied for producing zirconia/ceramic-veneer restorations. Bond strength values, measured by 3-point bending tests, were 34.42 ± 7.60 MPa for Group A and 31.92 ± 6.95 MPa for Group B. SEM observations of the cohesively fractured surfaces (on the porcelain side) and the examination for normality using the Shapiro-Wilk test suggested the use of Weibull statistical analysis. Median strength (σ50%) for Group A and Group B was 34.76 and 32.22 MPa, while the characteristic strength (σ63.2%) was 35.78 and 33.14 MPa, respectively. The Weibull modulus disparity between groups (12.69 and 13.07) was not significant. Bond strength exceeded the ISO 9693 minimum of 20 MPa, suggesting satisfactory strength for clinical use.

Microstructure, physical and mechanical properties of dental polychromic multilayer zirconia of uniform composition.

The present study aimed to compare the microstructure, physical, and mechanical properties of three commercially available dental polychromatic multilayer zirconia materials of uniform composition: Dima Mill Zirconia ML, VITA YZ/ST Multicolor, and VITA YZ/XT Multicolor (with 3, 4, and 5 mol% Y2 O3 , respectively); thus, the influence of Y2 O3 content on the above properties of the produced materials was experimentally studied. Homogeneous zirconia ceramics with a dense micro- and nanostructure, without pores or defects, were produced after milling the blocks and sintering, which resulted in yttrium-stabilized tetragonal and cubic zirconia. Statistical analysis of the results of measurable magnitudes was performed by the one-way ANOVA test. The increase of Y2 O3 content (from 3 to 5 mol%) favored larger grain and crystallite sizes and a decrease of the values of the mechanical properties; yet, the differences were statistically insignificant. Clinically, these differences are expected to have no impact on their function in the oral cavity, both in terms of their fracture propensity and the damage that can be caused to the opposing teeth. Accordingly, the experimental results qualify the polychromic multilayer zirconia ceramics of uniform composition fabricated by milling technology for use in dental restorations.

Synthesis, Structure-Property Evaluation and Biological Assessment of Supramolecular Assemblies of Bioactive Glass with Glycyrrhizic Acid and Its Monoammonium Salt.

Medical nutrients obtained from plants have been used in traditional medicine since ancient times, owning to the protective and therapeutic properties of plant extracts and products. Glycyrrhizic acid is one of those that, apart from its therapeutic effect, may contribute to stronger bones, inhibiting bone resorption and improving the bone structure and biomechanical strength. In the present study, we investigated the effect of a bioactive glass (BG) addition to the structure-property relationships of supramolecular assemblies formed by glycyrrhizic acid (GA) and its monoammonium salt (MSGA). FTIR spectra of supramolecular assemblies evidenced an interaction between BG components and hydroxyl groups of MSGA and GA. Moreover, it was revealed that BG components may interact and bond to the carboxyl groups of MSGA. In order to assess their biological effects, BG, MSGA, and their supramolecular assemblies were introduced to a culture of human bone-marrow-derived mesenchymal stromal cells (BMSCs). Both the BG and MSGA had positive influence on BMSC growth, viability, and osteogenic differentiation-these positive effects were most pronounced when BG1d-BG and MSGA were introduced together into cell culture in the form of MSGA:BG assemblies. In conclusion, MSGA:BG assemblies revealed a promising potential as a candidate material intended for application in bone defect reconstruction and bone tissue engineering approaches.

In Vivo Evaluation of 3D-Printed Silica-Based Bioactive Glass Scaffolds for Bone Regeneration.

Bioactive glasses are often designed as porous implantable templates in which newly-formed bone can grow in three dimensions (3D). This research work aims to investigate the bone regenerative capability of silicate bioactive glass scaffolds produced by robocasting in comparison with powder and granule-like materials (oxide system: 47.5SiO2-10Na2O-10K2O-10MgO-20CaO-2.5P2O5, mol.%). Morphological and compositional analyses performed by scanning electron microscopy (SEM), combined with energy dispersive spectroscopy (EDS) after the bioactivity studies in a simulated body fluid (SBF) confirmed the apatite-forming ability of the scaffolds, which is key to allowing bone-bonding in vivo. The scaffolds exhibited a clear osteogenic effect upon implantation in rabbit femur and underwent gradual resorption followed by ossification. Full resorption in favor of new bone growth was achieved within 6 months. Osseous defect healing was accompanied by the formation of mature bone with abundant osteocytes and bone marrow cells. These in vivo results support the scaffold's suitability for application in bone tissue engineering and show promise for potential translation to clinical assessment.

Biological Evaluation of a New Sodium-Potassium Silico-Phosphate Glass for Bone Regeneration: In Vitro and In Vivo Studies.

In vitro and in vivo studies are fundamental steps in the characterization of new implantable materials to preliminarily assess their biological response. The present study reports the in vitro and in vivo characterizations of a novel experimental silicate bioactive glass (BG) (47.5B, 47.5SiO2-10Na2O-10K2O-10MgO-20CaO-2.5P2O5 mol.%). Cytocompatibility tests were performed using human mature osteoblasts (U2OS), human mesenchymal stem cells (hMSCs) and human endothelial cells (EA.hy926). The release of the early osteogenic alkaline phosphatase (ALP) marker suggested strong pro-osteogenic properties, as the amount was comparable between hMSCs cultivated onto BG surface and cells cultivated onto polystyrene control. Similarly, real-time PCR revealed that the osteogenic collagen I gene was overexpressed in cells cultivated onto BG surface without biochemical induction. Acute toxicity tests for the determination of the median lethal dose (LD50) allowed classifying the analyzed material as a slightly toxic substance with LD50 = 4522 ± 248 mg/kg. A statistically significant difference in bone formation was observed in vivo through comparing the control (untreated) group and the experimental one, proving a clear osteogenic effect induced by the implantation at the defect site. Complete resorption of 47.5B powder was observed after only 3 months in favor of newly formed tissue, thus confirming the high osteostimulatory potential of 47.5B glass.

Synthesis of Silver Modified Bioactive Glassy Materials with Antibacterial Properties via Facile and Low-Temperature Route.

There is an increasing clinical need to develop novel biomaterials that combine regenerative and biocidal properties. In this work, we present the preparation of silver/silica-based glassy bioactive (ABG) compositions via a facile, fast (20 h), and low temperature (80 °C) approach and their characterization. The fabrication process included the synthesis of the bioactive glass (BG) particles followed by the surface modification of the bioactive glass with silver nanoparticles. The microstructural features of ABG samples before and after exposure to simulated body fluid (SBF), as well as their ion release behavior during SBF test were evaluated using infrared spectrometry (FTIR), ultraviolet-visible (UV-Vis) spectroscopy, X-ray diffraction (XRD), electron microscopies (TEM and SEM) and optical emission spectroscopy (OES). The antibacterial properties of the experimental compositions were tested against Escherichia coli (E. coli). The results indicated that the prepared ABG materials possess antibacterial activity against E. coli, which is directly correlated with the glass surface modification.

Mechanical and Biocompatibility Properties of Calcium Phosphate Bioceramics Derived from Salmon Fish Bone Wastes.

Natural calcium phosphates derived from fish wastes are a promising material for biomedical application. However, their sintered ceramics are not fully characterized in terms of mechanical and biological properties. In this study, natural calcium phosphate was synthesized through a thermal calcination process from salmon fish bone wastes. The salmon-derived calcium phosphates (sCaP) were sintered at different temperatures to obtain natural calcium phosphate bioceramics and then were investigated in terms of their microstructure, mechanical properties and biocompatibility. In particular, this work is concerned with the effects of grain size on the relative density and microhardness of the sCaP bioceramics. Ca/P ratio of the sintered sCaP ranged from 1.73 to 1.52 when the sintering temperature was raised from 1000 to 1300 °C. The crystal phase of all the sCaP bioceramics obtained was biphasic and composed of hydroxyapatite (HA) and tricalcium phosphate (TCP). The density and microhardness of the sCaP bioceramics increased in the temperature interval 1000-1100 °C, while at temperatures higher than 1100 °C, these properties were not significantly altered. The highest compressive strength of 116 MPa was recorded for the samples sintered at 1100 °C. In vitro biocompatibility was also examined in the behavior of osteosarcoma (Saos-2) cells, indicating that the sCaP bioceramics had no cytotoxicity effect. Salmon-derived biphasic calcium phosphates (BCP) have the potential to contribute to the development of bone substituted materials.

Dolomite-Foamed Bioactive Silicate Scaffolds for Bone Tissue Repair.

The use of three-dimensional (3D) scaffolds is recognized worldwide as a valuable biomedical approach for promoting tissue regeneration in critical-size bone defects. Over the last 50 years, bioactive glasses have been intensively investigated in a wide range of different clinical applications, from orthopedics to soft tissue healing. Bioactive glasses exhibit the unique capability to chemically bond to the host tissue and, furthermore, their processing versatility makes them very appealing due to the availability of different manufacturing techniques for the production of porous and interconnected synthetic bone grafts able to support new tissue growth over the whole duration of the treatment. As a novel contribution to the broad field of scaffold manufacturing, we report here an effective and relatively easy method to produce silicate glass-derived scaffolds by using, for the first time in the biomedical field, dolomite powder as a foaming agent for the formation of 3D bone-like porous structures. Morphological/structural features, crystallization behavior, and in vitro bioactivity in a simulated body fluid (SBF) were investigated. All the tested scaffolds were found to fulfil the minimum requirements that a scaffold for osseous repair should exhibit, including porosity (65-83 vol.%) and compressive strength (1.3-3.9 MPa) comparable to those of cancellous bone, as well as hydroxyapatite-forming ability (bioactivity). This study proves the suitability of a dolomite-foaming method for the production of potentially suitable bone grafts based on bioactive glass systems.

Effect of Alumina Incorporation on the Surface Mineralization and Degradation of a Bioactive Glass (CaO-MgO-SiO2-Na2O-P2O5-CaF2)-Glycerol Paste.

This study investigates the dissolution behavior as well as the surface biomineralization in simulated body fluid (SBF) of a paste composed of glycerol (gly) and a bioactive glass in the system CaO-MgO-SiO2-Na2O-P2O5-CaF2 (BG). The synthesis of the bioactive glass in an alumina crucible has been shown to significantly affect its bioactivity due to the incorporation of aluminum (ca. 1.3-1.4 wt %) into the glass network. Thus, the kinetics of the hydroxyapatite (HA) mineralization on the glass prepared in the alumina crucible was found to be slower than that reported for the same glass composition prepared in a Pt crucible. It is considered that the synthesis conditions lead to the incorporation of small amount of aluminum into the BG network and thus delay the HA mineralization. Interestingly, the BG-gly paste was shown to have significantly higher bioactivity than that of the as-prepared BG. Structural analysis of the paste indicate that glycerol chemically interacts with the glass surface and strongly alter the glass network architecture, thus generating a more depolymerized network, as well as an increased amount of silanol groups at the surface of the glass. In particular, BG-gly paste features early intermediate calcite precipitation during immersion in SBF, followed by hydroxyapatite formation after ca. seven days of SBF exposure; whereas the HA mineralization seems to be suppressed in BG, probably a consequence of the incorporation of aluminum into the glass network. The results obtained within the present study reveal the positive effect of using pastes based on bioactive glasses and organic carriers (here alcohols) which may be of interest not only due to their advantageous visco-elastic properties, but also due to the possibility of enhancing the glass bioactivity upon surface interactions with the organic carrier.

Understanding the Formation of CaAl2Si2O8 in Melilite-Based Glass-Ceramics: Combined Diffraction and Spectroscopic Studies.

An assessment is undertaken for the formation of anorthite crystalline phase in a melilite-based glass composition (CMAS: 38.7CaO-9.7MgO-12.9Al2O3-38.7SiO2 mol %), used as a sealing material in solid oxide fuel cells, in view of the detrimental effect of anorthite on the sealing properties. Several advanced characterization techniques are employed to assess the material after prolonged heat treatment, including neutron powder diffraction (ND), X-ray powder diffraction (XRD), 29Si and 27Al magic-angle spinning nuclear magnetic resonance (MAS-NMR), and in situ Raman spectroscopy. ND, 29Si MAS-NMR, and 27Al MAS-NMR results revealed that both Si and Al adopt tetrahedral coordination and participate in the formation of the network structure. In situ XRD measurements for the CMAS glass demonstrate the thermal stability of the glass structure up to 850 °C. Further heat treatment up to 900 °C initiates the precipitation of melilite, a solid solution of akermanite/gehlenite crystalline phase. Qualitative XRD data for glass-ceramics (GCs) produced after heat treatment at 850 °C for 500 h revealed the presence of anorthite along with the melilite crystalline phase. Rietveld refinement of XRD data indicated a high fraction of glassy phase (∼67%) after the formation of crystalline phases. The 29Si MAS-NMR spectra for the CMAS-GC suggest the presence of structural units in the remaining glassy phase with a polymerization degree higher than dimer units, whereas the 27Al MAS-NMR spectra revealed that most Al3+ cations exhibit a 4-fold coordination. In situ Raman spectroscopy data indicate that the formation of anorthite crystalline phase initiated after 240 h of heat treatment at 850 °C owing to the interaction between the gehlenite crystals and the remaining glassy phase.

Structure, biodegradation behavior and cytotoxicity of alkali-containing alkaline-earth phosphosilicate glasses.

We report on the effect of sodium on the structure, chemical degradation and bioactivity of glasses in the CaO-MgO-SiO2-P2O5-CaF2 system. The (29)Si and (31)P magic angle spinning-nuclear magnetic resonance spectroscopy of melt-quenched glasses with varying Na2O/MgO ratios exhibit a silicate glass network with the dominance of Q(2)(Si) units and phosphorus mainly forming orthophosphate species. Sodium incorporation in the glasses did not induce a significant structural change in the silicate network, while it did influence the phosphate environment due to its lower ionic field strength in comparison with that of magnesium. The apatite forming ability of glasses has been investigated by immersion of glass powders in simulated body fluid (SBF) for time durations varying between 1h and 7 days while their chemical degradation has been studied in Tris-HCl in accordance with ISO-10993-14. Increasing Na(+)/Mg(2+) ratio caused a decrease in the chemical durability of glasses and in the apatite forming ability especially during initial steps of interaction between glass and SBF solution. The cellular responses were observed in vitro on bulk glass samples using mouse-derived pre-osteoblastic MC3T3-E1 cell line. The preliminary study suggested that the increasing alkali-concentration in glasses led to cytotoxicity in the cell culture medium.

Structural analysis and thermal behavior of diopside-fluorapatite-wollastonite-based glasses and glass-ceramics.

Glass-ceramics in the diopside (CaMgSi2O6)-fluorapatite (Ca5(PO4)3F)-wollastonite (CaSiO3) system are potential candidates for restorative dental and bone implant materials. The present study describes the influence of varying SiO2/CaO and CaF2/P2O5 molar ratio on the structure and thermal behavior of glass compositions in the CaO-MgO-SiO2-P2O5-Na2O-CaF2 system. The structural features and properties of the glasses were investigated by nuclear magnetic resonance (NMR), infrared spectroscopy, density measurements and dilatometry. Sintering and crystallization behavior of the glass powders were studied by hot-stage microscopy and differential thermal analysis, respectively. The microstructure and crystalline phase assemblage in the sintered glass powder compacts were studied under non-isothermal heating conditions at 825 °C. X-ray diffraction studies combined with the Rietveld-reference intensity ratio (R.I.R) method were employed to quantify the amount of amorphous and crystalline phases in the glass-ceramics, while scanning electron microscopy was used to shed some light on the microstructure of resultant glass-ceramics. An increase in CaO/SiO2 ratio degraded the sinterability of the glass powder compacts, resulting in the formation of akermanite as the major crystalline phase. On the other hand, an increase in P2O5/CaF2 ratio improved the sintering behavior of the glass-ceramics, while varying the amount of crystalline phases, i.e. diopside, fluorapatite and wollastonite.

A new model formulation of the SiO2-Al2O3-B2O3-MgO-CaO-Na2O-F glass-ceramics.

Mono-phase glass-ceramics of akermanite were successfully produced from a Ca-mica and wollastonite via low-temperature sintering and crystallization. Doping with P(2)O(5) considerably improves sintering behaviour since P(2)O(5) increases the stability of glass against crystallization at the temperature of sintering onset. The resulting glass-ceramics feature good in vitro acceptance from osteoblasts, and moderate bioactivity due to the enrichment of the glassy phase with Ca and Si. The good quality of the white colour at the surface and throughout the bulk, the matching of microhardness with tooth enamel, and the possibility to coat other biomaterials such as ZrO(2), Ti or hydroxyapatite make these materials promising for medical applications.