Accuracy of additively manufactured zirconia four-unit fixed dental prostheses fabricated by stereolithography, digital light processing and material jetting compared with subtractive manufacturing.

OBJECTIVE: To evaluate the manufacturing accuracy of zirconia four-unit fixed dental prostheses (FDPs) fabricated by three different additive manufacturing technologies compared with subtractive manufacturing. METHODS: A total of 79 zirconia FDPs were produced by three different manufacturing technologies, representing additive (one stereolithography [aSLA] and one material jetting [aMJ] device, two digital light processing [aDLP1/aDLP2] devices) and subtractive manufacturing (two devices [s1/s2]), the latter serving as references. After printing, additively manufactured FDPs were debound and finally sintered. Subsequently, samples were circumferentially digitized and acquired surface areas were split in three Regions Of Interest (ROIs: inner/outer shell, margin). Design and acquired data were compared for accuracy using an inspection software. Statistical evaluation was performed using the root mean square error (RMSE) and nonparametric Kruskal-Wallis method with post hoc Wilcoxon-Mann-Whitney U tests. Bonferroni correction was applied in case of multiple testing. RESULTS: Regardless the ROI, significant differences were observed between manufacturing technologies (P < 0.001). Subtractive manufacturing was the most accurate with no significant difference regarding the material/device (s1/s2, P > 0.054). Likewise, no statistical difference regarding accurary was found when comparing s2 with aMJ and aSLA in most ROIs (P > 0.085). In general, mean surface deviation was< 50 µm for s1/s2 and aMJ and< 100 µm for aSLA and aDLP2. aDLP1 showed surface deviations> 100 µm and was the least accurate compared to the other additive/subtractive technologies. SIGNIFICANCE: Additive manufacturing represents a promising set of technologies for the manufacturing of zirconia FDPs, but not yet as accurate as subtractive manufacturing. Methodological impact on accuracy within and in between different additive technologies needs to be further investigated.

Passive sampling of environmental DNA in aquatic environments using 3D-printed hydroxyapatite samplers.

The study of environmental DNA (eDNA) released by aquatic organisms in their habitat offers a fast, noninvasive and sensitive approach to monitor their presence. Common eDNA sampling methods such as water filtration and DNA precipitation are time-consuming, require difficult-to-handle equipment and partially integrate eDNA signals. To overcome these limitations, we created the first proof of concept of a passive, 3D-printed and easy-to-use eDNA sampler. We designed the samplers from hydroxyapatite (HAp samplers), a natural mineral with a high DNA adsorption capacity. The porous structure and shape of the samplers were designed to optimize DNA adsorption and facilitate their handling in the laboratory and in the field. Here we show that HAp samplers can efficiently collect genomic DNA in controlled set-ups, but can also collect animal eDNA under controlled and natural conditions with yields similar to conventional methods. However, we also observed large variations in the amount of DNA collected even under controlled conditions. A better understanding of the DNA-hydroxyapatite interactions on the surface of the samplers is now necessary to optimize eDNA adsorption and to allow the development of a reliable, easy-to-use and reusable eDNA sampling tool.

Histologic and histomorphometric evaluation of new zirconia-based ceramic dental implants: A preclinical study in dogs.

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 split-mouth 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 < 0.05) was performed to compare peri-implant quantitative histomorphometric parameters on buccal and lingual sides, including Bone to Implant Contact (BIC) among test groups and time-periods. RESULTS: Titanium and ceramic implants presented respectively moderate and minimal roughness. After 4 and 13 weeks, ceramic implants showed an inflammatory tissue response close to titanium implants. At both period of time there was no significant difference between the titanium and ceramic groups in terms of BIC values (mean ± SD) at the lingual or buccal sides or when combining buccal + lingual BIC values (respectively for titanium and ceramic, 68.4 ± 14.7 % and 75.0 ± 13.5 % at 4 weeks, and 92.0 ± 8.6 % and 86.1 ± 13.8 % at 13 weeks). SIGNIFICANCE: Within the limits of the present study, it can be concluded that newly developed zirconia-based ceramic composite dental implants have similar biocompatibility and osseointegration to those observed in titanium implants. These pre-clinical results corroborate the potential for the use of these new zirconia-based ceramics in oral implantology.

High-translucent yttria-stabilized zirconia ceramics are wear-resistant and antagonist-friendly.

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.

Trade-off between fracture resistance and translucency of zirconia and lithium-disilicate glass ceramics for monolithic restorations.

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.

Mechanical behaviour of extremely tough TZP bioceramics.

Tetragonal Zirconia Polycrystals (TZP) is attractive for structural biomedical applications because of their excellent mechanical properties at room-temperature, which include high strength, fracture toughness and wear resistance. In this work, zirconia stabilized with Y or Yb or Yb+Nd, all containing 0.5 vol.% Al2O3, were prepared by hot-pressing (HP) at 50-60 MPa and sintered at 1300-1350 °C for 1 h. Microstructural features, phase composition and mechanical properties were investigated. The strength was measured by 4-point bending (4P-B), piston-on-three-balls (P-3B) and three-balls-on-three-balls (3B-3B) biaxial methods. Toughness was determined by indentation strength in bending (ISB). Vickers hardness (Hv) and the Young modulus (E) were also estimated. Preliminary aging behaviour (LTD) was also here considered. Measured biaxial strength was significantly higher (until 1.83 times) than the uniaxial one because of the tetragonal to monoclinic (t-m) zirconia phase transformation which is strongly influenced by the loading configuration. The variation of the strength with the testing method is attributed to the compressive stresses generated by the phase transformation which is particularly favoured under P-3B tests and also to the calculation of the stresses from elastic theories. LTD preliminary tests showed excellent aging resistance of 3Yb-0.5A ceramics.

Towards long lasting zirconia-based composites for dental implants: Transformation induced plasticity and its consequence on ceramic reliability.

Zirconia-based composites were developed through an innovative processing route able to tune compositional and microstructural features very precisely. Fully-dense ceria-stabilized zirconia ceramics (84vol% Ce-TZP) containing equiaxed alumina (8vol%Al2O3) and elongated strontium hexa-aluminate (8vol% SrAl12O19) second phases were obtained by conventional sintering. This work deals with the effect of the zirconia stabilization degree (CeO2 in the range 10.0-11.5mol%) on the transformability and mechanical properties of Ce-TZP-Al2O3-SrAl12O19 materials. Vickers hardness, biaxial flexural strength and Single-edge V-notched beam tests revealed a strong influence of ceria content on the mechanical properties. Composites with 11.0mol% CeO2 or above exhibited the classical behaviour of brittle ceramics, with no apparent plasticity and very low strain to failure. On the contrary, composites with 10.5mol% CeO2 or less showed large transformation-induced plasticity and almost no dispersion in strength data. Materials with 10.5mol% of ceria showed the highest values in terms of biaxial bending strength (up to 1.1GPa) and fracture toughness (>10MPa√m). In these ceramics, as zirconia transformation precedes failure, the Weibull modulus was exceptionally high and reached a value of 60, which is in the range typically reported for metals. The results achieved demonstrate the high potential of using these new strong, tough and stable zirconia-based composites in structural biomedical applications. STATEMENT OF SIGNIFICANCE: Yttria-stabilized (Y-TZP) zirconia ceramics are increasingly used for developing metal-free restorations and dental implants. Despite their success related to their excellent mechanical resistance, Y-TZP can undergo Low Temperature Degradation which could be responsible for restoration damage or even worst the failure of the implant. Current research is focusing on strategies to improve the LTD resistance of Y-TZP or to develop alternative composites with better stability in vivo. In this work the mechanical characterization of a new type of very-stable zirconia-based composites is presented. These materials are composed of ceria-stabilized zirconia (84vol%Ce-TZP) containing two second phases (α-alumina and strontium hexa-aluminate) and exhibit exceptional strength, toughness and ductility, which may allow the processing of dental implants with a perfect reliability and longer lifetime.

Effect of loading configuration on strength values in a highly transformable zirconia-based composite.

OBJECTIVES: The aim of this work was to determine mechanical properties of a highly transformable 10Ce-TZP/Al2O3/La2AlO3 composite, currently developed as a biomaterial for dental application, and to investigate the effect of loading configuration on its flexural strength. METHODS: Fracture toughness is determined by the single-edge-V-notched beam (SEVNB) method. Strength measurements were conducted by four-point bending and biaxial bending tests (piston-on-three balls) according to ISO 6872, dedicated to ceramic materials in dentistry. RESULTS: Strength obtained by either four-point or biaxial bending are very different, and take the values of 596MPa and 1470MPa respectively. It is demonstrated that the difference in measured strength cannot be attributed to the effect of volume on strength, generally predicted by the standard Weibull analysis, but to different transformation behaviors for the two bending configurations. More extensive transformation occurs in the biaxial configuration, with a lower autocatalytic transformation stress threshold, resulting to substantial compressive residual stresses. SIGNIFICANCE: The significant influence of the loading configuration on the strength should be integrated when designing a component from a highly transformable ceramic.

Towards long lasting zirconia-based composites for dental implants. Part I: innovative synthesis, microstructural characterization and in vitro stability.

In order to fulfill the clinical requirements for strong, tough and stable ceramics used in dental applications, we designed and developed innovative zirconia-based composites, in which equiaxial α-Al2O3 and elongated SrAl12O19 phases are dispersed in a ceria-stabilized zirconia matrix. The composite powders were prepared by an innovative surface coating route, in which commercial zirconia powders were coated by inorganic precursors of the second phases, which crystallize on the zirconia particles surface under proper thermal treatment. Samples containing four different ceria contents (in the range 10.0-11.5 mol%) were prepared by carefully tailoring the amount of the cerium precursor during the elaboration process. Slip cast green bodies were sintered at 1450 °C for 1 h, leading to fully dense materials. Characterization of composites by SEM and TEM analyses showed highly homogeneous microstructures with an even distribution of both equiaxial and elongated-shape grains inside a very fine zirconia matrix. Ce content plays a major role on aging kinetics, and should be carefully controlled: sample with 10 mol% of ceria were transformable, whereas above 10.5 mol% there is negligible or no transformation during autoclave treatment. Thus, in this paper we show the potential of the innovative surface coating route, which allows a perfect tailoring of the microstructural, morphological and compositional features of the composites; moreover, its processing costs and environmental impacts are limited, which is beneficial for further scale-up and real use in the biomedical field.

Surface Coating of Oxide Powders: A New Synthesis Method to Process Biomedical Grade Nano-Composites.

Composite and nanocomposite ceramics have achieved special interest in recent years when used for biomedical applications. They have demonstrated, in some cases, increased performance, reliability, and stability in vivo, with respect to pure monolithic ceramics. Current research aims at developing new compositions and architectures to further increase their properties. However, the ability to tailor the microstructure requires the careful control of all steps of manufacturing, from the synthesis of composite nanopowders, to their processing and sintering. This review aims at deepening understanding of the critical issues associated with the manufacturing of nanocomposite ceramics, focusing on the key role of the synthesis methods to develop homogeneous and tailored microstructures. In this frame, the authors have developed an innovative method, named "surface-coating process", in which matrix oxide powders are coated with inorganic precursors of the second phase. The method is illustrated into two case studies; the former, on Zirconia Toughened Alumina (ZTA) materials for orthopedic applications, and the latter, on Zirconia-based composites for dental implants, discussing the advances and the potential of the method, which can become a valuable alternative to the current synthesis process already used at a clinical and industrial scale.

Synthesis and thermal behaviour of nanostructured ZrO2 powders obtained under hydrothermal conditions.

Nanocrystalline zircone (ZrO2) powders were synthesized from zirconium oxyacetate aqueous solution treated up to 240 degrees C under autogeneous pressure. Depending on experimental conditions, colloidal particles of 26-150 nm are formed by aggregation of zirconia crystallites. The effect of some experimental conditions over the colloidal particle size or zirconia phase composition was studied. The powder sintering behaviour is also presented.

Supercritical fluid technology of nanoparticle coating for new ceramic materials.

This work highlights, for the first time, the coating of ferroelectric nanoparticles with a chemical fluid deposition process in supercritical fluids. BaTiO3 nanoparticles of about 50 nm are coated with a shell of a few nanometers of amorphous alumina and can be recovered as a dry powder for processing. The sintering of these core-shell nanoparticles gives access to a ceramic material with very interesting ferroelectric properties, in particular, dielectric losses below 1%.