Synthesis and characterization of poly(vinyl alcohol)/chondroitin sulfate composite hydrogels containing strontium-doped hydroxyapatite as promising biomaterials.

Novel poly(vinyl alcohol)/chondroitin sulfate (PVA/CS) composite hydrogels containing hydroxyapatite (HA) or Sr-doped HA (HASr) particles were synthesized by a freeze/thaw method and characterized aiming towards biomedical applications. HA and HASr were synthesized by a wet-precipitation method and added to the composite hydrogels in fractions up to 15 wt%. Physical-chemical characterizations of particles and hydrogels included scanning electron microscopy, energy-dispersive spectroscopy, Fourier-transform infrared spectroscopy, X-ray diffraction, thermogravimetry, porosity, compressive strength/elastic modulus, swelling degree, and cell viability. Particles were irregular in shape and appeared to have narrow size variation. The thermal behavior of composite hydrogels was altered compared to the control (bare) hydrogel. All hydrogels exhibited high porosity. HA/HASr particles reduced total porosity without reducing pore size. The mechanical strength was improved as the fraction of HA or HASr was increased. HASr particles led to a faster water uptake but did not interfere with the total hydrogel swelling capacity. In cell viability essay, increased cell growth (above 120%) was observed in all groups including the control hydrogel, suggesting a bioactive effect. In conclusion, PVA/CS hydrogels containing HA or HASr particles were successfully synthesized and showed promising morphological, mechanical, and swelling properties, which are particularly required for scaffolding.

Non-silicate nanoparticles for improved nanohybrid resin composites.

OBJECTIVE: Zirconia and alumina nanoparticles were coated with a silica-rich layer (ALSI and ZRSI) and used to prepare experimental nanohybrid resin composites, which were characterized and compared to a control commercial resin composite (Filtek Z350 XT). METHODS: Silica nanoparticles with sizes compatible to ALSI (Aerosil 150) and ZRSI (Aerosil OX 50) were tested as references. The volume of nanoparticles was equivalent across the composites, which also had consistent content of glass microparticles. CC conversion, viscosity, depth of cure, surface topography, hardness, opacity, radio-opacity, and edge chipping resistance (ReA) were tested after 24 h. Flexural strength (σf) and fracture toughness (KIC) were also tested after 15 K thermal cycles. Data were analyzed using one-way or two-way ANOVA and Tukey's test (α = 0.05). RESULTS: ALSI and ZRSI yielded resin composites with lower viscosity and more irregular nanoagglomerates compared to nanosilica-based composites. CC conversion and depth of cure were lower for ZRSI composite, which had higher opacity, radio-opacity, and hardness. ReA was higher for ALSI composite. Composites with ALSI and ZRSI showed stable σf after aging, whereas the control and Aerosil 150 resin composites showed significant degradation. The commercial and nanosilica-based composites showed up to 42% reduction in KIC after aging, whereas resin composites with ZRSI and ALSI showed a more stable KIC. SIGNIFICANCE: ALSI and ZRSI generated nanohybrid resin composites with improved and/or more stable physical properties compared with nanosilica-based and commercial composites. This study suggests that changing the composition of nanofillers is a simple method to enhance the performance of nanohybrid composites.

The progressive wear and abrasiveness of novel graded glass/zirconia materials relative to their dental ceramic counterparts.

OBJECTIVE: To investigate the wear behavior of novel graded glass/zirconia materials and their abrasiveness to the antagonist relative to homogeneous zirconias (polished or glazed) and a glass-ceramic. METHODS: Graded glass/zirconia specimens were prepared by sintering with concurrent glass-infiltration of pre-sintered zirconia (3Y-TZP) with a polished or as-machined surface. Monolithic zirconia samples were sintered and their surfaces were polished or glazed (as-machined). Glass-ceramic samples were obtained and the surface polished. All specimens were subjected to chewing simulations with a steatite antagonist (r = 3 mm) and a cyclic load of 50 N. Quantitative measurements of wear and roughness were performed on ceramics and antagonists for prescribed number of cycles. Damage sustained in ceramics and antagonists was analyzed by SEM. RESULTS: The polished zirconia presented little to no variation in wear depth (2 µm) and roughness (0.06 µm). Graded and glazed zirconia experienced a rapid increase in wear depth while the superficial glass layer was present (until 1000 cycles), but showed little variations afterwards - at 450k cycles ∼15 µm for graded and 78 µm for glazed zirconia. The glass-ceramic presented the greatest wear depth (463 µm) and roughness (1.48 µm). Polished zirconia, polished graded zirconia and glazed zirconia yielded significantly lower volumetric wear (∼3 mm3) of the antagonist than as-machined graded zirconia and glass-ceramic (∼5 mm3). SIGNIFICANCE: Polished graded zirconia and polished zirconia presented little wear and roughness, as well as yielded reduced antagonist wear. Glassy materials are both more susceptible to wear and more abrasive to the antagonist relative to zirconia.

Synthesis of silver-containing calcium aluminate particles and their effects on a MTA-based endodontic sealer.

OBJECTIVE: To synthetize calcium aluminate (C3A) and silver-containing C3A particles (C3A+Ag) testing their effects on the properties of a MTA-based endodontic sealer in comparison to an epoxy resin- and a calcium silicate-based sealer. METHODS: Pure C3A and C3A+Ag particles were synthesized by a chemical method and characterized using XRD to identify crystalline phases. SEM/EDS analysis investigated morphology, particle size, and elemental composition of particles. Setting time, flow, radiopacity, water sorption and solubility of commercial and modified sealers were evaluated according to ISO 6876/2012. The pH and ions release were measured using a pHmeter and a microwave induced plasma optical emission spectrometer. The inhibition of biofilm growth was evaluated by confocal laser scanning microscopy (CLSM). Data were rank transformed and analyzed by ANOVA and Tukey test (P<0.05). RESULTS: The C3A particles showed an irregular grain agglomerated structure with voids and pores. In C3A+Ag particles, Ag modified the material morphology, confirming the deposition of Ag. The physicochemical properties of the modified MTA-based sealer were similar to the commercial material, except for the significant increase in Ca+2 release. However, there was no Ag release. Setting time, flow, radiopacity, water sorption and solubility were adequate for all materials. All the materials showed alkaline pH. Antibiofilm effect was improved in the presence of C3A particles, while the biofilm inhibition was lower in the presence of Ag. SIGNIFICANCE: The modified sealer presented improved antibiofilm properties and calcium release, without dramatic effects on the other characteristics. It is expected a positive effect in its antimicrobial behavior.

Speed sintering translucent zirconia for chairside one-visit dental restorations: Optical, mechanical, and wear characteristics.

The fabrication of zirconia dental restorations is a time-consuming process due to traditional slow sintering schemes; zirconia (Y-TZP) produced by these conventional routes are predominantly opaque. Novel speed sintering protocols have been developed to meet the demand for time and cost effective chairside CAD/CAM-produced restorations, as well as to control ceramic microstructures for better translucency. Although the speed sintering protocols have already been used to densify dental Y-TZP, the wear properties of these restorations remain elusive. Fast heating and cooling rates, as well as shorter sintering dwell times are known to affect the microstructure and properties of zirconia. Thus, we hypothesize that speed sintered zirconia dental restorations possess distinct wear and physical characteristics relative to their conventionally sintered counterparts. Glazed monolithic molar crowns of translucent Y-TZP (inCoris TZI, Sirona) were fabricated using three distinct sintering profiles: Super-speed (SS, 1580 °C, dwell time 10 min), Speed (S, 1510 °C, dwell time 25 min), and Long-term (LT, 1510 °C, dwell time 120 min). Microstructural, optical and wear properties were investigated. Crowns that were super-speed sintered possessed higher translucency. Areas of mild and severe wear were observed on the zirconia surface in all groups. Micropits in the wear crater were less frequent for the LT group. Groups S and SS exhibited more surface pits, which caused a scratched steatite surface that is associated with a greater volume loss. Tetragonal to monoclinic phase transformation, resulting from the sliding wear process, was present in all three groups. Although all test groups had withstood thermo-mechanical challenges, the presence of hairline cracks emanating from the occlusal wear facets and extending deep into the restoration indicates their susceptibility to fatigue sliding contact fracture.

Functionalized pink Al2O3:Mn pigments applied in prosthetic dentistry.

STATEMENT OF PROBLEM: The color of dental poly(methyl methacrylate) (PMMA) is conventionally rendered by organic and inorganic pigments, which are usually not bonded to the polymer network. Functionalized ceramic pigments can be used to color PMMA, allowing improved chemical interaction with the resin matrix. PURPOSE: The purpose of this in vitro study was to synthesize, functionalize, and characterize pink manganese-doped alumina ceramic pigments. The hypothesis tested was that functionalized ceramic pigments would render pink coloration to a translucent PMMA without jeopardizing its mechanical properties. MATERIAL AND METHODS: Pink alumina powders doped with 1 or 2 mol% of manganese (Al2O3:Mn) were prepared by means of a polymeric precursor method. Pigment (Pig.) particles were functionalized with a silica coating method followed by silanation before preparation of PMMA-based composite resins (5 wt% pigment). The color of composite resins (Pig.1% and Pig.2%) and PMMA controls (Pink and translucent [Trans]) was evaluated (CIELab color coordinates), and their mechanical properties were tested (3-point bending). RESULTS: The microstructure of the pigment particles showed approximately 55-nm nanocrystals of manganese-doped α-alumina clustered into irregular porous particles up to 60 µm. The composite resins and pink PMMA showed similar color parameters (CIE a* pink=20.1, Pig.1%=14.6, Pig.2%=16.0, Trans=0.19, P<.001; CIE b* Pink=17.0, Pig.1%=18.6, Pig.2%=19.0, Trans=2.52, P<.001). No statistical differences were observed in mechanical properties among groups (σf pink=98.4, Pig.1%=98.1, Pig.2%=98.8, trans=89.1, P=.136). CONCLUSIONS: The addition of the functionalized pink ceramic pigments to a translucent PMMA yielded similar coloration to that of the regular pink PMMA used in dentistry and did not jeopardize its mechanical properties.

Mono or polycrystalline alumina-modified hybrid ceramics.

OBJECTIVES: This study evaluated the effect of addition of alumina particles (polycrystalline or monocrystalline), with or without silica coating, on the optical and mechanical properties of a porcelain. METHODS: Groups tested were: control (C), polycrystalline alumina (PA), polycrystalline alumina-silica (PAS), monocrystalline alumina (MA), monocrystalline alumina-silica (MAS). Polycrystalline alumina powder was synthesized using a polymeric precursor method; a commercially available monocrystalline alumina powder (sapphire) was acquired. Silica coating was obtained by immersing alumina powders in a tetraethylorthosilicate solution, followed by heat-treatment. Electrostatic stable suspension method was used to ensure homogenous dispersion of the alumina particles within the porcelain powder. The ceramic specimens were obtained by heat-pressing. Microstructure, translucency parameter, contrast ratio, opalescence index, porosity, biaxial flexural strength, roughness, and elastic constants were characterized. RESULTS: A better interaction between glass matrix and silica coated crystalline particles is suggested in some analyses, yet further investigation is needed to confirm it. The materials did not present significant differences in biaxial flexural strength, due to the presence of higher porosity in the groups with alumina addition. Elastic modulus was higher for MA and MAS groups. Also, these were the groups with optical qualities and roughness closer to control. The PA and PAS groups were considerably more opaque as well as rougher. SIGNIFICANCE: Porcelains with addition of monocrystalline particles presented superior esthetic qualities compared to those with polycrystalline particles. In order to eliminate the porosity in the ceramic materials investigated herein, processing parameters need to be optimized as well as different glass frites should be tested.