In vitro performance of 2-step, total etch adhesives modified by thiourethane additives.

OBJECTIVES: Thio-urethane oligomeric additives have been shown to improve the mechanical properties of dental composites and resin cements. To try to harness those same properties in dental adhesives, in this study, these oligomers (TU) were added to the matrix and/or as filler functionalization of experimental adhesives, and the effects on conversion and mechanical properties were analyzed. METHODS: BisGMA and HEMA (60/40 wt%) were used as the monomer matrix, made polymerizable by the addition of 0.2 wt% 2,2-dimethoxy-2- phenylacetophenone. 2,6-di-tert-butyl-4-methylphenol was added at 0.5 wt% as the inhibitor. This material was used as the unfilled control (BH). TU oligomers were added at 20 wt % to the matrix (BH+20%TU, unfilled) and/or used as filler functionalization (TF, 10 wt%). Fillers functionalized with methacrylate (MF, 10 wt%) served as the control. The experimental adhesives groups containing fillers were: BH+10%MF; BH+10%TF; BH+20%TU+10%MF; BH+20%TU+10%TF. Flexural properties were tested in three-point bending (wet and dry). Polymerization kinetics was followed in real-time in near-IR. Water Sorption/Solubility (WS/SL, ISO 4049) and Viscosity (rotational rheometry) were also evaluated. For Microtensile bond strength 40 vol% ethanol was added to adhesives, which was applied onto sound dentin from third human molars. The data were analyzed with one-way ANOVA and Tukey post-hoc test, and test t for the comparison between storage time of the microtensile bond strength test (alpha = 0.05). RESULTS: There was no significant difference between groups when yield strength (YS) and flexural modulus (FM) were evaluated in dry conditions. After water storage, all the groups containing TU in the matrix showed statistically lower YS/FM values. This was true in spite of the statistically higher conversion for those same groups. The maximum rate of polymerization (Rpmax) was higher for BH+10%TF and no significant difference was found for the groups BH and BH+10% MF. The lowest Rpmax values were found for BH+20%TU+10%TF and BH+20%TU. BH+20%TU+10%TF showed the highest viscosity values followed by BH+20%TU+10%MF and BH+20%TU, with statistically significant difference between them. For the microtensile bond strength test at 24h (p = 0.13) and 6 months (p = 0.11) and WS/SL (p > 0.05), no significant difference was found among groups. The storage time (24 h and 6 months) did not affect the microtensile bond strength results. CONCLUSION: In spite of improving the conversion, the addition of TU in the matrix reduced the mechanical properties of the adhesives tested after water storage. This did not affect the bond strength at 24 h or 6 months.

Evaluation of Cleaning Methods on Lithium Disilicate Glass Ceramic Surfaces After Organic Contamination.

The purposes of this study were to 1) evaluate the effectiveness of different cleaning methods from a previously etched and silanized lithium disilicate glass ceramic (EMX) surface after contact with organic fluids (saliva or human blood) and 2) assess the effect of applying a new silane layer after the cleaning methods on the microshear bond strength (mSBS) of resin cement to EMX. EMX discs were etched with 5% hydrofluoric acid (HF) and properly silanized. Three control groups were created (n=10): control (without contamination), saliva positive, and human blood positive. Later, after new contaminations, the samples were distributed into four groups according to the cleaning method (n=20): air-water spray (AWS), 35% phosphoric acid, 70% alcohol, or Ivoclean cleaning paste. After the cleaning methods, subgroups were submitted to a new silane layer application, or not (n=10). All samples received a thin layer of a bonding agent and, subsequently, three light-cured resin cement cylinders were prepared on each EMX surface for the mSBS test. This test was performed on a universal testing machine at a vertical speed of 1 mm/minute until rupture. Contaminated and cleaned silanized EMX surfaces were assessed by scanning electron microscopy (SEM) (n=1). The noncontaminated control group showed an average mSBS of 18.7 MPa, and the positive saliva and human blood control groups yielded a 34% and 42% reduction in bond strength, respectively, compared to the uncontaminated control (p<0.05). For saliva-contaminated surfaces, all cleaning methods were effective and not different from one another or the control group (p>0.05). However, for human blood contamination, only Ivoclean cleaning paste was effective in restoring µSBS to uncontaminated control group levels (p>0.05). SEM images showed a clean surface (ie, with no contaminant residues) after the cleaning methods, regardless of the organic contaminant type. All the assessed cleaning methods were effective in removing saliva from the silanized EMX surface; however, only Ivoclean was able to restore the adhesion quality when the silanized EMX surface was contaminated with human blood.

Effect of Hydrofluoric Acid Concentration and Etching Time on Bond Strength to Lithium Disilicate Glass Ceramic.

The aim of this study was to evaluate the influence of different concentrations of hydrofluoric acid (HF) associated with varied etching times on the microshear bond strength (µSBS) of a resin cement to a lithium disilicate glass ceramic. Two hundred seventy-five ceramic blocks (IPS e.max Press [EMX], Ivoclar Vivadent), measuring 8 mm × 3 mm thickness, were randomly distributed into five groups according to the HF concentrations (n=50): 1%, 2.5%, 5%, 7.5%, and 10%. Further random distribution into subgroups was performed according to the following etching times (n=10): 20, 40, 60, 120, and 20 + 20 seconds. After etching, all blocks were treated with a silane coupling agent followed by a thin layer of an unfilled resin. Three resin cement cylinders (∅=1 mm) were made on each EMX surface, which was then stored in deionized water at 37°C for 24 hours before testing. The µSBS was in a universal testing machine at a crosshead speed of 1 mm/min until failure. Data were submitted to two-way analysis of variance, and multiple comparisons were performed using the Tukey post hoc test (α=0.05). One representative EMX sample was etched according to the description of each subgroup and evaluated using scanning electron microscopy for surface characterization. The HF concentrations of 5%, 7.5%, and 10% provided significantly higher µSBS values than 1% and 2.5% (p<0.05), regardless of the etching times. For 1% and 2.5% HF, the etching times from 40 to 120 seconds increased the µSBS values compared with 20 seconds (p<0.05), but etching periods did not differ within the 5%, 7.5%, and 10% HF groups (p>0.05). The effect of re-etching was more evident for 1% and 2.5% HF (p<0.05). Different HF concentrations/etching times directly influenced the bond strength and surface morphology of EMX.