Comparison of marginal adaptation and internal fit of monolithic lithium disilicate crowns produced by 4 different CAD/CAM systems.

OBJECTIVES: To evaluate the marginal adaptation and internal space of crowns produced by 4 CAD/CAM systems using microcomputed tomography (µCT) and replica technique (RT). MATERIALS AND METHODS: Monolithic lithium disilicate crowns were milled (Ceramill, Cerec, EDG, and Zirkonzahn) (n = 10). The cement film obtained with low viscosity silicone was scanned by the µCT system and captured by a stereomicroscope, according to RT. Two-way ANOVA followed by Tukey's test were used for statistical analysis (α = 0.05). A uniformity index (UI) was idealized to describe the distribution of crowns' internal space and submitted to the Kruskal-Wallis and Tukey's test (α = 0.05). The correlation between µCT and RT was performed by Pearson's Correlation Coeficient (α = 0.05). RESULTS: Marginal adaptation and internal space were statistically significant different between the experimental groups for the µCT and RT (p < 0.05). The medians of the 4 systems tested were within clinically acceptable range and the mean (± SD) highest marginal discrepancy was recorded in the Ceramill group at 133.0 ± 71.5 µm (µCT) and 90.6 ± 38.5 µm (RT). For internal fit, the UI disclosed a better distribution of the internal space for the Zirkonzahn group (p < 0.001). There was a strong correlation between the methods (p = 0.01 and r = 0.69). CLINICAL RELEVANCE: Because of the variability of the CAD/CAM systems available, evaluating their accuracy is of clinical interest. The 4 systems are capable to produce restorations adaptated within clinically appropriate levels. The µCT and RT are efficient adaptation methodologies.

Translucency parameter of conventional restorative glass-ionomer cements.

OBJECTIVE: To evaluate the translucency parameter (TP) and contrast ratio (CR) of different conventional restorative glass-ionomer cements (GICs). MATERIALS AND METHODS: Eighteen brands of GICs were evaluated. Five disks of each material were made following ISO 9917-1. The luminous reflectance and Central Bureau of the International Commission on Illumination parameters of disks were evaluated using a colorimeter, against backings of white and black, to obtain the translucent parameter and contrast ratio of different brands of glass-ionomer cements. The correlation between translucency parameter and contrast ratio was assessed with the Pearson correlation test. The translucent and contrast ratio parameters values were submitted to the one-way ANOVA and Tukey test for multiple comparisons (p < 0.05). RESULTS: There was a strong inverse relationship between CR and TP (r2  = 0.94, p < 0.001). The contrast ratio decreased as translucency increased. There were significant differences in TP and CR among brands (p < 0.001). CONLUSIONS: GICs exhibit different translucency and contrast ratio behavior. Some brands of GICs presented very low TP and this condition would be unacceptable for areas with esthetic demands. In addition, TP and CR showed a strong linear relationship. CLINICAL SIGNIFICANCE: The results found in this study demonstrated that the knowledge of the translucency and CR of different conventional restorative GICs is important in order to guide clinicians in the selection of restorative GICs for anterior teeth.

Influence of thickness and aging on the mechanical properties of provisional resin materials.

This study aimed to evaluate the flexural strength (FS) and modulus of elasticity (ME) of 2 provisional resins at different thicknesses and after different storage periods. A total of 80 specimens were made of 2 provisional restorative materials (n = 40): Dencôr (DC) or Protemp 4 (PT). The specimens in each material group were prepared in 2 different thicknesses (n = 20): 1.5 mm or 2.0 mm. The groups were further subdivided by storage time (n = 10 per material thickness per time): 7 days or 3 months. A 3-point bending test was performed with a universal testing machine. Data were submitted to 3-way analysis of variance followed by a post hoc Tukey test (α = 0.05). Regarding the interaction of material and thickness, the 2.0-mm-thick DC specimens presented a significantly lower mean FS (41.08 MPa) than the other groups (P < 0.05). Regarding the interaction of material and storage time, PT after 3 months presented a significantly higher mean FS (75.51 MPa) than the other groups and periods (P < 0.05). Regardless of the material, the highest mean ME was found in the 1.5-mm-thick group after 3 months (2.24 GPa) (P < 0.05). The lowest ME values were found in the 2.0-mm-thick specimens after both storage times (7 days, 0.88 GPa; 3 months, 1.09 GPa), which were not significantly different from each other (P > 0.05). The correlation between FS and ME was direct and positive (R2 = 0.51; P < 0.001), independently of the variables (material, thickness, and time). Therefore, 2.0-mm-thick PT specimens presented the highest values of FS, mainly after 3 months. The ME was higher after 3 months (1.5-mm-thick specimens), regardless of the material. In addition, the higher the FS, the higher the ME of the material.

Impact of the intermediary layer on sealant retention: a randomized 24-month clinical trial.

OBJECTIVES: The aims of this study were to assess long-term impact of tooth eruption stages (ES) on sealant retention on occlusal surfaces previously coated with intermediary bonding layer and to determine caries prevention. MATERIALS AND METHODS: Sixty-five school children were selected (aged 6-10 years), with four non-carious permanent first molar in different ES (OP (operculum present), ME (marginal edge), CE (completely erupted)). Split-mouth and single-blind study design was used. The teeth (260) were randomly selected according to treatment (sealant/technique): F (Fluroshield), H (Helioseal Clear Chroma), SF (Single Bond + F), EH (Excite + H). Sealant retention, marginal integrity, discoloration, and caries prevention were assessed after 6, 12, 18, and 24 months by calibrated examiner (Spearman = 0.91) using visual inspection. Data were submitted to the Cox proportional hazard model (survival analysis) and Likelihood ratio χ 2 test (correlation), p ≤ 0.05. RESULTS: At baseline, ES was 20 % in OP, 54 % in ME, and 26 % in CE. There was no significant difference on sealant retention between the treatments (p = 0.2774). However, significant differences were found regarding the ES on sealant retention (p = 0.0041). The CE stage showed the highest retention survival rate during the 24 months. The overall sealant prevention average was found to be about 99.4 % and showed no difference between the groups. CONCLUSIONS: Eruption stages affect sealant retention irregardless of the intermediate layer and type of sealant. However, there was caries prevention on tooth occlusal surfaces after 24 months, regardless of treatment. CLINICAL RELEVANCE: Sealing is recommended to prevent occlusal caries of newly erupted teeth in high-caries-risk patients. However, its application is critical on moisture limited control surfaces independently of sealer material and technique.

Role of chlorhexidine in bond strength to artificially eroded dentin over time.

PURPOSE: To assess the long-term effect of a 2% aqueous chlorhexidine (CHX) solution on bond strength to artificially eroded dentin compared to sound dentin. MATERIALS AND METHODS: Flat mid-coronal dentin surfaces of extracted third molars (n = 28) were subjected only to grinding with a 600-grit SiC paper for 1 min (sound dentin S, n = 14) or additionally to erosive pH cycling with a cola-based soft-drink (eroded dentin E, n = 14). After acid etching, rinsing, and air drying, S and E were rehydrated with 1.5 µl of 2% CHX (S2%, n = 7; E2%, n = 7) or of distilled water (control SC, n = 7; EC, n = 7). Composite buildups were incrementally constructed with Filtek Z350 following Adper Single Bond 2 application. Specimens were sectioned into beams, which were subjected to microtensile testing immediately or after 6 or 12 months of aging. Fractured surfaces were observed under a digital microscope (50X magnification). Microtensile bond strength (µTBS) (MPa) was analyzed by three-way ANOVA and Tukey's tests (α = 0.05) and failure mode by the Kruskal-Wallis test (α = 0.05). RESULTS: Compared to sound dentin, eroded dentin was consistently related to lower µTBS. Immediately and after 12-month aging, the effect of CHX was insignificant, but it was significant after 6-month aging, when it conserved the bond strength to both eroded and sound dentin. The percentage of adhesive and mixed failures were equivalent, and significantly more frequent than cohesive failures, whether in dentin or in composite. CONCLUSION: The 2% CHX effect on bond strength conservation to both eroded and sound dentin was not found to be persistent.

Stress Distribution in Single Dental Implant System: Three-Dimensional Finite Element Analysis Based on an In Vitro Experimental Model.

This study aimed to analyze the stress distribution in single implant system and to evaluate the compatibility of an in vitro model with finite element (FE) model. The in vitro model consisted of Brånemark implant; multiunit set abutment of 5 mm height; metal-ceramic screw-retained crown, and polyurethane simulating the bone. Deformations were recorded in the peri-implant region in the mesial and distal aspects, after an axial 300 N load application at the center of the occlusal aspect of the crown, using strain gauges. This in vitro model was scanned with micro CT to design a three-dimensional FE model and the strains in the peri-implant bone region were registered to check the compatibility between both models. The FE model was used to evaluate stress distribution in different parts of the system. The values obtained from the in vitro model (20-587 µÎµ) and the finite element analysis (81-588 µÎµ) showed agreement among them. The highest stresses because of axial and oblique load, respectively were 5.83 and 40 MPa for the cortical bone, 55 and 1200 MPa for the implant, and 80 and 470 MPa for the abutment screw. The FE method proved to be effective for evaluating the deformation around single implant. Oblique loads lead to higher stress concentrations.

Photo-crosslinkable hydrogel incorporated with bone matrix particles for advancements in dentin tissue engineering.

The objective of this study was to create injectable photo-crosslinkable biomaterials, using gelatin methacryloyl (GelMA) hydrogel, combined with a decellularized bone matrix (BMdc) and a deproteinized (BMdp) bovine bone matrix. These were intended to serve as bioactive scaffolds for dentin regeneration. The parameters for GelMA hydrogel fabrication were initially selected, followed by the incorporation of BMdc and BMdp at a 1% (w/v) ratio. Nano-hydroxyapatite (nHA) was also included as a control. A physicochemical characterization was conducted, with FTIR analysis indicating that the mineral phase was complexed with GelMA, and BMdc was chemically bonded to the amide groups of gelatin. The porous structure was preserved post-BMdc incorporation, with bone particles incorporated alongside the pores. Conversely, the mineral phase was situated inside the pore opening, affecting the degree of porosity. The mineral phase did not modify the degradability of GelMA, even under conditions of type I collagenase-mediated enzymatic challenge, allowing hydrogel injection and increased mechanical strength. Subsequently, human dental pulp cells (HDPCs) were seeded onto the hydrogels. The cells remained viable and proliferative, irrespective of the GelMA composition. All mineral phases resulted in a significant increase in alkaline phosphatase activity and mineralized matrix deposition. However, GelMA-BMdc exhibited higher cell expression values, significantly surpassing those of all other formulations. In conclusion, our results showed that GelMA-BMdc produced a porous and stable hydrogel, capable of enhancing odontoblastic differentiation and mineral deposition when in contact with HDPCs, thereby showing potential for dentin regeneration.

Are we approaching the development of a novel calcium phosphate-based bioceramic dental material?

OBJECTIVES: Develop a sustainable bovine hydroxyapatite dental ceramic with the addition of titanium dioxide (TiO2) nanoparticles (5 % and 8 % by weight), analyzing the outcome of this addition to the microstructure, as well as its mechanical and chemical properties, in order to evaluate whether they satisfy the International Organization for Standardization (ISO) 6872:2015 for dental ceramics or not. METHODS: Disks were obtained through uniaxial followed by isostatic pressing from bovine hydroxyapatite powder and TiO2 nanoparticles and sintered at 1300ºC for 2 h. Three experimental groups were developed (HA, HA+5 %TiO2 and HA+8 %TiO2) and subjected to X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), indentation fracture (IF), biaxial flexural strength (BFS) and chemical solubility test. RESULTS: XRD revealed, for HA group, the appearance of a peak corresponding to b-tricalcium phosphate (ß-TCP). For HA+ 5 %TiO2 and HA+ 8 %TiO2, the entire composition was converted into ß-TCP and calcium titanate (CaTiO3). The SEM images showed a dense ceramic matrix and a uniform distribution of another phase in groups with TiO2 nanoparticles. HA+ 5 %TiO2 (1.40 ± 0.18 MPa.m1/2) and HA+ 8 %TiO2 (1.32 ± 0.18 MPa.m1/2) showed significantly higher fracture toughness values than HA (0.67 ± 0.09 MPa.m1/2). HA showed significantly higher characteristic stress (295.8 MPa) in comparison to groups with 5 % (235.1 MPa) and 8 % (214.4 MPa) TiO2 nanoparticles. Differences were not observed between the Weibull modulus values. The solubility results indicated that all experimental ceramics were above the 2000 ug/cm2 limit set by the ISO 6872:2015. SIGNIFICANCE: This study proposed the development and characterization of a new ceramic for dental prosthesis made from HA extracted from bovine bones, with the intention of reusing these solids waste and transforming them into a sustainable and low-cost material. Although the experimental calcium phosphate ceramic with additions of 5 % and 8 % of TiO2 achieved desirable mechanical properties, the chemical solubility values were very high.

A new technique for incorporation of TiO2 nanotubes on a pre-sintered Y-TZP and its effect on bond strength as compared to conventional air-borne particle abrasion and silicatization TiO2 nanotubes application on pre-sintered Y-TZP.

OBJECTIVE: This study evaluated the microshear bond strength of a resin cement to Y-TZP after different methods of TiO2 nanotubes (nTiO2) incorporation on pre-sintered Y-TZP surfaces. METHODS: nTiO2 were synthesized and incorporated on Y-TZP slices as follows (n = 15): 1) nTiO2 mixed with isopropyl alcohol/manual application (MAl); 2) nTiO2 mixed with acetone/manual application (MAc); 3) nTiO2 mixed with isopropyl alcohol/high-pressure vacuum application (HPVAl); 4) nTiO2 mixed with acetone/high-pressure vacuum application (HPVAc). As controls, surfaces were sandblasted with Al2O3 (OX) or Rocatec silicatization (ROC). All ceramics were sintered after nTiO2 incorporation. Surface treatments of OX and ROC were made after sintering. Surfaces were characterized by confocal laser microscopy, scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS). Resin composite cylinders (1.40 mm diameter and 1 mm height) were cemented with a resin cement, stored in water at 37 °C for 24 h and thermocycled for 10 000 cycles before microshear bond strength evaluation. Data were analyzed with one-way ANOVA and Games-Howell (α = 0.05), and fracture analysis was performed using a stereomicroscope. RESULTS: EDS confirmed the presence of TiO2 on treated Y-TZP. The confocal analysis showed higher roughness for HPVAc and OX. There were significant differences between surface treatments (p < 0.001). HPVAl (22.96 ± 10.3), OX (34.16 ± 7.9) and ROC (27.71 ± 9.4) showed higher microshear bond strengths and were statistically similar (p > 0.05). MAC showed intermediary values, and HPVAc and MAl presented decreased bond strength, with a high percentage of premature debonding. CONCLUSION: High-pressure vacuum application of nTiO2 mixed with isopropyl alcohol was able to produce bond strength values compared to conventional air abrasion and Rocatec silicatization. SIGNIFICANCE: The infiltration of TiO2 nanostructures on the pre-sintered Y-TZP is an interesting approach that can improve bond strength without the need of sandblasting methods.

Resin-based materials to control human dentin permeability under erosive conditions in vitro: A hydraulic conductance, confocal microscopy and FTIR study.

OBJECTIVES: To characterize the behavior of three different polymeric agents before and after an erosive challenge on dentin permeability, to analyze their degradation in both conditions, and to analyze their degree of conversion (DC). METHODS: The permeability of human dentin disks (1.0 ± 0.2 mm) was measured with smear layer, after its removal, after treatment (LpTreat) with Gluma Desensitizer, PRG Barrier Coat (PBC) or Icon infiltrant (n = 11/group) and after exposure to citric acid (LpEro) (6%, pH 2.1, 1 min). The specimens were analyzed under a Laser Scanning Confocal Microscope (n = 2/group) and the products' DC were calculated. Data were subjected to 2-way repeated measures ANOVA and post-hoc Bonferroni (permeability analysis), to paired t-test (for specimens treated with Icon) and to t-test (DC analysis) (α < 0.05). RESULTS: Icon showed the lowest LpTreat and LpEro values, while PBC and Gluma did not differ from each other under these conditions. Icon and PBC showed LpEro similar to a dentin with smear layer. Under the Laser Scanning Confocal Microscope, more deposits were noticeable on dentin after treating with PBC. Gluma presented the deepest penetration in dentin. The DC of PBC was the highest. SIGNIFICANCE: Icon caused the highest reduction on permeability values, followed by PBC and Gluma. PBC generated more deposits covering dentin and seemed to be more efficient after an erosive challenge. The association of a polymeric resin with inorganic ion-releasing fillers seem to be a great strategy to manage dentin hypersensitivity under erosive conditions.

Y-TZP Physicochemical Properties Conditioned with ZrO2 and SiO2 Nanofilms and Bond Strength to Dual Resin Cement.

Commercial Yttria-tetragonal zirconia polycrystalline (Y-TZP) was subjected to surface treatments, and the bond strength of dual resin cement to Y-TZP and failure modes were evaluated. Disks (12 mm × 2 mm), cylinders (7 mm × 3.3 mm), and bars (25 mm × 5 mm × 2 mm) were milled from Y-TZP CAD-CAM blocks, divided into seven groups, and subjected to different surface treatments; silicatization was used as control. On the basis of the literature, this study evaluated modifications with films containing SiO2 nanoparticles and silane; SiO2+ZrO2­SiO2 (50%) and ZrO2 (50%) nanoparticles, SiO2+ZrO2/Silane-SiO2 (50%) and ZrO2 (50%) nanoparticles, and silane. Specimens were analyzed by wettability (n = 3), surface free energy (n = 3), X-ray diffraction (n = 1), Fourier transform infrared spectroscopy (FTIR) (n = 1), roughness (n = 5), shear bond test (n = 10), and dynamic modulus (n = 3). Specimens treated with hydrofluoric acid­HF 40% presented significantly higher contact angle and lowest surface free energy (p < 0.05). The SiO2/Silane presented crystalline SiO2 on the surface. The surface roughness was significantly higher for groups treated with nanofilms (p < 0.05). Shear bond strength was significantly higher for silicatization, HF 40%/silicatization, SiO2/Silane, and SiO2+ZrO2/Silane groups. The proposed treatments with nanofilms had potentially good results without prejudice to the physicochemical characteristics of zirconia. Generally, groups that underwent silica surface deposition and silanization had better bond strength (p < 0.005).

TiO2 nanoparticles added to dense bovine hydroxyapatite bioceramics increase human osteoblast mineralization activity.

OBJECTIVES: This study evaluated the effect of TiO2 nanoparticles + dense hydroxyapatite (HA) on human osteoblast cells (SAOS-2). METHODS: Particulate bovine HA powder with or without the addition of either 5 or 8 % TiO2 (HA, HA/TiO2Np5 % or HA/TiO2Np8 %) were pressed into disks (Ø = 12.5 mm; thickness = 1.3 mm) uniaxially (100 MPa) and isostatically (200 MPa/1 min) and sintered at 1300 °C. Y-TZP disks were used as control. The following tests were performed: Scanning Electron Microscopy and Dispersive Energy Spectroscopy (SEM/EDS), Atomic Force Microscopy (AFM), cell viability assay (Alamar Blue-AB) and mineralized matrix deposition (Alizarin Red-AR). AB and AR data were submitted to 2-way ANOVA/Tukey tests and ANOVA/Tukey tests, respectively. RESULTS: SEM revealed that the surface of HA/TiO2Np5% resembles DPBHA surface, but also contains smaller granules. HA/TiO2Np8% characteristics resembles HA/TiO2Np5% surface, but with irregular topography. Y-TZP showed a typical oxide ceramic surface pattern. EDS revealed Ca, O, and P in all samples. C, O, and Zr appeared in Y-TZP samples. AFM data corroborates SEM analysis. AB test revealed excellent cellular viability for HA/TiO2Np5% group. AR test showed that all groups containing TiO2np had more mineralized matrix deposition than all other groups, with statistically differences between HA/TiO2Np8% and HA cultivated in non-osteogenic medium. Culture in osteogenic medium exhibited much more mineralized matrix deposition by TiO2np groups. SIGNIFICANCE: In conclusion, the addition of TiO2np showed chemical, superficial, and biological changes in the reinforced materials. HA/TiO2Np5% showed the best results for cell viability and HA/TiO2Np8% for mineralized matrix deposition.

Effect of TiF4 varnish after pre-treatment with proanthocyanidin or chlorhexidine on the progression of erosive dentin loss in the presence or absence of the demineralized organic matrix.

This study evaluated the protective effect of TiF4 varnish, after pre-treatment with proantocyanidin or chlorhexidine, on the progression of erosive dentin loss (EDL), under the presence or absence of the demineralized organic matrix (DOM). Bovine root dentin samples were eroded for 30 min (0.1% citric acid, pH 2.5) and the loss was measured by profilometry. Half of them were subjected to the DOM removal using collagenase for 4 days, while the other half remained immersed in water. The removal of DOM was checked by profilometry. Samples were divided into 24 groups (n = 15) according to the factors: 1- With or without DOM; 2- Pre-treatment with 0.012% chlorhexidine gel, 10% proanthocyanidin gel or untreated for 1 min; 3-Final Treatment with TiF4 varnish, NaF varnish, placebo varnish or untreated for 6 h. The samples were submitted to a pH cycling for 5 days: 0.1% citric acid (4 × 90s/day) and artificial saliva between the challenges. The final profile was obtained for the calculation of EDL (µm, three-way ANOVA/Tukey test). When DOM was preserved, the EDL was lower compared to the condition without DOM (7.08 ± 4.03 µm and 9.80 ± 3.79 µm, p < 0.001, respectively), regardless of the treatments. The pre-treatment had no influence on the progression of EDL (p = 0.637), while the final treatment (TiF4 varnish only, 6.77 ± 4.08 µm) was effective in reducing the progression of EDL (NaF varnish: 9.52 ± 4.02 µm; Placebo varnish: 8.64 ± 4.06 µm and no treatment: 8.80 ± 3.95 µm). It can be concluded that DOM has important protective effect on the progression of EDL. TiF4 was the unique treatment capable of reducing EDL progression, regardless of the pre-treatment of DOM.

Consensus on glass-ionomer cement thresholds for restorative indications.

OBJECTIVE: The aim of this paper is to present the results of a consensus meeting on the threshold property requirements for the clinical use of conventional glass-ionomer cements (GICs) for restorative indications. METHODS: Twenty-one experts on GICs evaluated the results of tests on mechanical and optical properties of 18 different brands of restorative GICs: Bioglass R [B], Chemfil Rock [CR], Equia Forte [EF], Gold Label 2 [GL2], Gold Label 9 [GL9], Glass Ionomer Cement II [GI], Ionglass [IG], Ion Z [IZ], Ionomaster [IM], Ionofil Plus [IP], Ionostar Plus [IS], Ketac Molar Easymix [KM], Magic Glass [MG], Maxxion R [MA], Riva Self Cure [R], Vidrion R [V], Vitro Fil [VF] and Vitro Molar [VM]. All experiments were carried out by a team of researchers from Brazil and England following strict protocols, under the same laboratory conditions throughout, and maintaining data integrity. RESULTS: There was consensus on: determining as primary properties of the material: compressive strength, microhardness, acid erosion and fluoride release, and as secondary properties: contrast ratio and translucency parameter, in order to rank the materials. Seven brands were below the thresholds for restorative indications: IZ, IM, IG, MA, VF, B and MG. CONCLUSIONS: Based on the primary properties adopted as being essential for restorative indications, the conventional restorative GICs that met the thresholds and could be considered suitable as long-term restorative materials were: EF, GI, GL9, KM, IP, GL2, IS, CR, V, VM and R. A decision-making process to select the best GIC must also include results from clinical trials. CLINICAL SIGNIFICANCE: This study provides a ranking of GICs that could be considered suitable as long-term restorative materials based on their main properties.

Effect of the addition of functionalized TiO2 nanotubes and nanoparticles on properties of experimental resin composites.

OBJECTIVE: To evaluate the influence of the addition of functionalized and non-functionalized TiO2 nanostructures on properties of a resin composite. METHODS: TiO2 nanostructures were synthesized and functionalized, using 3-(aminopropyl)triethoxysilane (APTMS) and 3-(trimethoxysilyl)propyl methacrylate (TSMPM). Characterizations were performed with XRD, EDS, TEM, and TGA. Resin composites containing Bis-GMA/TEGDMA, CQ, DABE, and barium-aluminum silicate glass were produced according to TiO2 nanostructure (nanotube or nanoparticle), concentration (0.3 or 0.9 wt%), and functionalization (APTMS or TSMPM). The resin composite without nanostructures was used as control. The amount of fillers was kept constant at 78.3 wt% for all materials. The degree of conversion (DC - at 0 h and 24 h), maximum polymerization rate (Rpmax), and Knoop microhardness (KHN before and after ethanol softening) were evaluated. Data were analyzed with two-way ANOVA with repeated measures and Tukey's HSD (α = 0.05). RESULTS: TGA results demonstrated that functionalizations were effective for both nanostructures. For DC, resin composites, time and interaction effect were significant (p < 0.001). Higher DC was found for 0.3-wt%-functionalized-nanotubes at 24 h. For nanoparticles, only 0.9-wt%-non-functionalized and 0.3-wt%-APTMS-functionalized showed DC similar to the control and all other groups showed higher DC (p < 0.05). Rpmax was higher for 0.3-wt%-APTMS-nanotubes, which corresponded to higher DC after 24 h. The lowest Rpmax occurred for 0.9-wt%-TSMPM-nanotubes, which showed smaller DC at 0 h. For KHN, resin composites, ethanol softening and interaction effect were significant (p < 0.001). KHN decreased after ethanol softening all groups, except for 0.3-wt%-TSMPM-nanotubes, 0.9-wt%-TSMPM-nanotubes, and 0.3-wt%-non-functionalized-nanoparticles. CONCLUSION: The resin with 0.3-wt%-TSMPM-nanotubes showed higher DC after 24 h, while being the most stable material after the ethanol softening. SIGNIFICANCE: The addition of functionalized TiO2 nanostructures in resin-based materials may improve the properties of the material.

Effects of ZnO/TiO2 nanoparticle and TiO2 nanotube additions to dense polycrystalline hydroxyapatite bioceramic from bovine bones.

OBJECTIVES: A bovine dense hydroxyapatite ceramic (HA) was produced as new biomaterial, however, the production of a material with consistently high flexural strength remains challenging. The objective of this study was to evaluate the effects of ZnO nanoparticles, TiO2 nanoparticles, and TiO2 nanotubes (1%, 2%, and 5% by weight) on the microstructure and flexural strength of a bovine dense hydroxyapatite ceramic (HA). METHODS: Discs (Ø=12.5mm; thickness=1.3mm) were prepared and subjected to X-ray diffraction (XRD), and observation with a field emission scanning electron microscope (FE-SEM), biaxial flexural strength (BFS) testing, and Vickers hardness (VH) testing. The BFS and VH data were subjected to ANOVA and Tukey post-hoc tests (α=0.05) and Weibull analysis. RESULTS: The XRD showed that the addition of nanomaterials caused the formation of a secondary phase when 5% of the ZnO nanoparticles was used, or when all percentages of the TiO2 nanoparticles/nanotubes were used, and the HA crystallographic planes were maintained. Differences were not observed between the higher BFS values obtained with pure HA and those obtained with the 5% addition of TiO2 nanoparticles. However, the results were different compared with the other groups (α=0.05). The results obtained by Weibull analysis revealed that the 1%, 2%, and 5% addition of TiO2 nanotubes, and the 1% and 2% addition of TiO2 nanoparticles decreased the HA characteristic strength (σ0), while the Weibull modulus (m) increased when 5% of TiO2 nanoparticles, 1% and 2% of ZnO nanoparticles, and 2% of TiO2 nanoparticles were added, but with no statistical difference from the pure HA. The 5% addition of ZnO2 nanoparticles decreased the σ0 without changing m. Moreover, the 5% addition of TiO2 nanoparticles resulted in an m closest to that of pure HA. Regarding the VH results, the blend of HA with 1% and 2% addition of TiO2 nanoparticles exhibited the higher values, which were similar between the different addition ratios (p=0.102). Moreover, the addition of 5% TiO2 nanoparticles resulted in higher value compared with pure HA. SIGNIFICANCE: This study demonstrated that the HA blend with 5% of TiO2 nanoparticles has the greatest potential as a bovine HA dense bioceramic reinforcement.

Correlation between mechanical properties and stabilization time of chemical bonds in glass-ionomer cements.

The objective was to evaluate the compressive strength (CS), diametral tensile strength (DTS), flexural strength (FS), and Knoop microhardness (KH) of different conventional restorative glass-ionomer cements (GICs) and to correlate these mechanical properties (MP) with the stabilization time (ST) of their chemical bonds. Eighteen GICs were tested: Bioglass [B], Chemfil Rock [CR], Equia Forte [EF], Gold Label 2 [GL2], Gold Label 9 [GL9], Glass Ionomer Cement II [GI], Ionglass [IG], Ion Z[ IZ], Ionomaster [IM], Ionofil Plus [IP], Ionostar Plus [IS], Ketac Molar Easymix [KM], Magic Glass [MG], Maxxion R [Ma], Riva Self Cure [R], Vidrion R [V], Vitro Fil [VF] and Vitro Molar [VM]. The mechanical strength tests were performed in a universal testing machine. KH readings were done with a diamond indenter. STs were examined by Fourier Transform Infrared spectroscopy (FTIR). Data were analyzed with ANOVA and Tukey test (p<0.05). The Spearman rank test was used to evaluate the dependence between the MPs and ST results. The highest MP values were EF, GL2, GL9, GI and KM and the lowest for MG, MA, B, VF and IM. The longest ST was for GL2 and the shortest was for B. ST correlated positively with MP. GICs with longer chemical bonds ST are generally stronger and the ST value obtained from FTIR was useful in predicting the strength of GICs tested.

Yttria-stabilized tetragonal zirconia polycrystal/resin luting agent bond strength: Influence of Titanium dioxide nanotubes addition in both materials.

PURPOSE: To evaluate the shear bond strength (SBS) between Y-TZP and a resin luting agent, after 1 of 2 enhancing strategies with TiO2--nts was applied, either to the resin luting agent or the Y-TZP mass, in different concentrations. METHODS: In the Strategy TiO2-nts on ceramic, the resin luting agent Panavia F2.0™ (Kuraray) and an experimental Y-TZP with added concentrations of TiO2--nts (0%, 1%, 2%, and 5% vol/vol) and a commercial Y-TZP, comprised 5 different groups (n = 10). In the Strategy TiO2-nts on cement, the resin luting agent RelyX U200™ (3 M ESPE) was added with different concentrations of TiO2--nts (0%, 0.3%, 0.6%, 0.9% wt/wt) luted to a commercial Y-TZP, comprising 4 different groups (n = 10). The Y-TZP discs were included in acrylic bases, and a cylinder (3 × 3 mm) of the correspondent luting agent for each respective group was applied over them. After 24 h, specimens were subjected to SBS assessments in a universal testing machine. Field emission scanning electron microscopy and energy dispersive X-ray spectroscopy analyses were also performed on Y-TZP surfaces. Data were analyzed via analysis of variance and Tukey tests (α = 0.05). RESULTS: TiO2-nts on ceramic influenced the bond strength significantly, but not linearly; TiO2-nts on cement did not influence bond strength when analyzed separately, nor in comparison with the first. CONCLUSION: Y-TZP enhancements with TiO2-nts led to a higher SBS with Panavia F2.0, a 5% TiO2--nt concentration presented the highest bond strength. Modified Rely X U200 did not improve SBS.

Aging resistant ZTA composite for dental applications: Microstructural, optical and mechanical characterization.

OBJECTIVE: To synthesize a zirconia toughened alumina (ZTA) composite with 70% alumina reinforced by 30% zirconia for dental applications and to characterize its microstructure and optical properties for comparison with the isolated counterpart materials and a first-generation 3Y-TZP. METHODS: Disc-shaped specimens were divided in four groups (n = 70/material): (1) 3YSB-E (first generation 3Y-TZP), (2) Zpex (second generation 3Y-TZP), (3) alumina, and (4) ZTA-Zpex 70/30. After synthesis, ceramic powders were pressed, and green-body samples sintered following a predetermined protocol. Specimens were polished to obtain a mirror surface finish. Apparent density was measured by Archimedes principle. X-ray diffraction (XRD) and scanning electron microscope (SEM) were used to characterize the crystalline content and microstructure. Reflectance tests were performed to determine the contrast-ratio (CR) and translucency-parameter (TP). Mechanical properties were assessed by biaxial flexural strength (BFS) test. All analyses were conducted before and after artificial aging (20 h, 134 °C, 2.2 bar). Optical parameters were evaluated through repeated-measures analysis of variance and Tukey tests (p < 0.05). BFS data were analyzed using Weibull statistics (95% CI). RESULTS: High density values (95-99%) were found for all ceramic materials and SEM images exhibited a dense microstructure. While XRD patterns revealed the preservation of crystalline content in the ZTA composite, an increase in the monoclinic peak was observed for pure zirconias after aging. Significantly higher CR and lower TP values were observed for the ZTA composite, followed by alumina, 3YSB-E, and Zpex. The highest characteristic stress was recorded for 3YSB-E, followed by intermediate values between ZTA and Zpex, and the lowest for alumina. Aging affected the optical and mechanical properties of both zirconias, while remained stable for ZTA composite and alumina. SIGNIFICANCE: The synthesis of experimental 70-30% ZTA composite was successful and its relevance for dental applications relies on its higher masking ability, aging resistance, and strength similar to zirconia.

TiO2 nanotubes improve physico-mechanical properties of glass ionomer cement.

OBJECTIVES: The aim of this study was to determine the physico-mechanical properties of a high viscosity glass ionomer cement (GIC) reinforced with TiO2 nanotubes (TiO2-nt). METHODS: TiO2-nt was incorporated into the GIC powder components (Ketac Molar EasyMix™) in concentrations of 0% (control group), 3%, 5%, 7% by weight. Compressive strength (n = 10/group), three point bending for flexural strength (n = 18/group), microshear bond strength to dentin and failure mode (n = 20/group), and surface roughness and weight loss before and after brushing simulation (30,000 cycles) (n = 8/group) were evaluated. Data were submitted to Shapiro-Wilk, ANOVA, Tukey and Chi-square tests (α ≤ 0.05). RESULTS: Addition of 5% of TiO2-nt into GIC presented the highest values for compressive strength and differed from the control, 3% and 7% groups (p = 0.023). There were no significant differences in flexural strength (p = 0.107) and surface roughness before and after the dental brushing (p = 0.287) among the groups. GIC added with 5% TiO2-nt showed the lowest weight loss values (p = 0.01), whereas the control, 3% or 5% TiO2-nt groups presented similar microshear bond strength values (p ≥ 0.05). The 5% TiO2-nt group featured higher microshear bond strength than the 7% TiO2-nt group (p = 0.034). Cohesive in material was the most representative failure mode for all groups. SIGNIFICANCE: The incorporation of TiO2-nt did not affect GIC's adhesiveness to dentin, but improved its compressive strength at 5%. Furthermore, TiO2-nt decreased the percentage of weight loss after GIC's surface wear.