Pong Pongprueksa

Dentin Bonding Testing Using a Mini-interfacial Fracture Toughness Approach

Measurement of interfacial fracture toughness (iFT) is considered a more valid method to assess bonding effectiveness as compared with conventional bond strength testing. Common fracture toughness tests are, however, laborious and require a relatively bulky specimen size. This study aimed to evaluate a new simplified and miniaturized iFT (mini-iFT) test. Four dentin adhesives, representing the main adhesive classes, and 1 glass ionomer cement were applied onto flat dentin. Mini-iFT (1.5 × 2.0 × 16 to 18 mm) and microtensile bond strength (µTBS; 1.5 × 1.5 × 16 to 18 mm) specimens were prepared from the same tooth. For the mini-iFT specimens, a single notch was cut at the adhesive-dentin interface with a 150-µm diamond blade under water cooling; the specimens were loaded until failure in a 4-point bending test setup. Finite element analysis was used to analyze stress distribution during mini-iFT testing. The correlation between the mean mini-iFT and µTBS was examined and found to be significant; a strong positive correlation was found (r2 = 0.94, P = 0.004). Weibull data analysis suggested the mini-iFT to vary less than the µTBS. Both the mini-iFT and the µTBS revealed the same performance order, with the 3-step etch-and-rinse adhesive outperforming the 2-step self-etch and 2-step etch-and-rinse adhesive, followed by the 1-step SE adhesive and, finally, the glass ionomer cement. Scanning electron microscopy failure analysis revealed the adhesive-dentin interface to fail more at the actual interface with the mini-iFT test, while µTBS specimens failed more within dentin and composite. This finding was corroborated by finite element analysis showing stress to concentrate at the interface during mini-iFT loading and crack propagation. In conclusion, the new mini-iFT test appeared more discriminative and valid than the µTBS to assess bonding effectiveness; the latter test nevertheless remains more versatile. Specimen size and workload were alike, making the mini-iFT test a valid alternative for the popular µTBS test.

Interfacial fracture toughness of aged adhesive-dentin interfaces.

OBJECTIVE To assess interfacial fracture toughness of different adhesive approaches and compare to a standard micro-tensile bond-strength (μTBS) test after 6 months water storage. METHODS Chevron-notched beam fracture toughness (CNB) was determined using a modified ISO 24370:2005 standard. Adhesive-dentin micro-specimens (1.0 mm × 1.0 mm × 8-10 mm) were stressed in tensile until failure to determine the micro-tensile bond strength (μTBS). RESULTS The highest mean μTBS and interfacial fracture toughness were measured for the multi-step adhesives Clearfil SE Bond (Kuraray Noritake) and OptiBond FL (Kerr). While large differences were observed in the bond strength values (from 7.4 to 27.2 MPa) of the one-step self-etch adhesives tested, interfacial fracture toughness was less different (from 0.7 to 1.0 MPam(1/2)). The adhesive with the lowest mean toughness (All-bond Universal, Bisco) had however the highest Weibull reliability, which might be a better parameter in regard to more consistent clinical performance. The self-adhesive composite Vertise Flow (Kerr) scored significantly lower at all levels. SIGNIFICANCE Although the ranking of the adhesives tested using CNB and μTBS corresponded well, the outcome of CNB appeared more reliable and less variable.

Influence of Light Irradiation Through Zirconia on the Degree of Conversion of Composite Cements

PURPOSE To assess the light irradiance (LI) delivered by two light-curing units and to measure the degree of conversion (DC) of three composite cements and one flowable composite when cured through zirconia or ceramic-veneered zirconia plates with different thicknesses. MATERIALS AND METHODS Three dual-curing composite cements (Clearfil Esthetic Cement, Panavia F2.0, G-CEM LinkAce) and one light-curing flowable composite (G-aenial Universal Flo) were investigated. Nine different kinds of zirconia plates were prepared from three zirconia grades (YSZ: Aadva and KATANA; Ce-TZP/Al2O3: NANOZR) in three different thicknesses (0.5- and 1.5-mm-thick zirconia, and 0.5-mm-thick zirconia veneered with a 1.0-mm-thick veneering ceramic). Portions of the mixed composite cements and the flowable composite were placed on a light spectrometer to measure LI while being light cured through the zirconia plates for 40 s using two light-curing units (n = 5). After light curing, micro-Raman spectra of the composite films were acquired to determine DC at 5 and 10 min, 1 and 24 h, and at 1 week. RESULTS The zirconia grade and the thickness of the zirconia/veneered zirconia plates significantly decreased LI. Increased LI did not increase DC. Only the Ce-TZP/Al2O3 (NANOZR) zirconia was too opaque to allow sufficient light transmission and resulted in significantly lower DC. CONCLUSION Although zirconia-based restorations attenuate the LI of light-curing units, the composite cements and the flowable composite could be light cured through the YSZ zirconia. LI is too low through Ce-TZP/Al2O3 zirconia, necessitating the use of self-/dual-curing composite cements.

Effect of Evaporation on the Shelf Life of a Universal Adhesive

OBJECTIVES The purpose of this study was to evaluate how evaporation affects the shelf life of a one-bottle universal adhesive. METHODS Three different versions of Scotchbond Universal (SBU, 3M ESPE, Seefeld, Germany) were prepared using a weight-loss technique. SBU0 was left open to the air until maximal weight loss was obtained, whereas SBU50 was left open until 50% of evaporation occurred. In contrast, SBU100 was kept closed and was assumed to contain the maximum concentration of all ingredients. The degree of conversion (DC) was determined by using Fourier transform infrared spectroscopy on different substrates (on dentin or glass plate and mixed with dentin powder); ultimate microtensile strength and microtensile bond strength to dentin were measured as well. RESULTS DC of the 100% solvent-containing adhesive (SBU100) was higher than that of the 50% (SBU50) and 0% (SBU0) solvent-containing adhesives for all substrates. DC of the adhesive applied onto glass and dehydrated dentin was higher than that applied onto dentin. Even though the ultimate microtensile strength of SBU0 was much higher than that of SBU50 and SBU100, its bond strength to dentin was significantly lower. CONCLUSIONS Evaporation of adhesive ingredients may jeopardize the shelf life of a one-bottle universal system by reducing the degree of conversion and impairing bond strength. However, negative effects only became evident after more than 50% evaporation.

Mini-interfacial fracture toughness as a new validated enamel-bonding effectiveness test.

UNLABELLED Today׳s most commonly applied bonding effectiveness tests are criticized for their high variability and low reliability, the latter in particular with regard to measuring the actual strength of the adhesive interface. OBJECTIVES in continuation of previous research conducted at dentin, we hereby aimed to validate the novel mini-interfacial fracture toughness (mini-iFT) test on its applicability to assess bonding effectiveness of contemporary adhesives when bonded to enamel. METHODS The 3-step etch&rinse (E&R) adhesive OptiBond FL (Kerr), the 2-step self-etch (SE) adhesive Clearfil SE Bond (Kuraray Noritake) and the two multi-mode adhesives Clearfil S(3) Bond Plus (Kuraray Noritake) and Scotchbond Universal (3M ESPE), both used following a 2-step E&R and 1-step SE mode, were applied to clinically relevant, flattened enamel surfaces. A composite (Filtek Z100; 3M ESPE) build-up was made in layers. After 1-week water storage at 37°C, all specimens were sectioned perpendicular to the interface to obtain rectangular sticks. A mini-iFT notch was prepared at the adhesive-enamel interface using a thin diamond blade under water cooling. Finally, the specimens were loaded in a 4-point bending test until failure. RESULTS the mini-iFT onto human enamel was significantly higher for the adhesives applied in E&R mode versus those applied in SE mode. The lowest mini-iFT was found for the adhesives applied following a 1-step SE approach. SEM fracture analysis revealed that all fractures originated at the adhesive-enamel interface and that the induced crack propagated preferentially along this interface. CONCLUSION mini-iFT appeared a valid alternative method to assess the mechanical properties of adhesive-enamel interfaces.

Response to Letter to the Editor, “Dentin Bonding Testing Using a Mini-interfacial Fracture Toughness Approach”:

In response to the letter to the editor by Ruse (2016), we confirm that the finite element modeling dimensions were similar to those of the actually tested specimens; the depicted model in Figure 1 is shorter in order to detail the loaded part. During initial loading, stress was not entirely uniformly distributed but concentrated at the actual adhesive-dentin interface (Appendix Fig. 1c, d). Once the crack propagated, stress uniformly distributed (Appendix Fig. 1e, f). Scanning electron microscopy confirmed a parallel crack progression, also witnessed by the observed hackle. We assume that nonuniform stress distribution would have led to premature failures—and, hence, lower values—while our values are higher than those previously reported, though not that substantially, considering the range reported in the review by Söderholm (2010): 1–4 MPa·m and 1–2 MPa·m for dentin and interface specimens, respectively (standard deviations often exceeding 25%). Despite the strongly expressed urge for an interfacial fracture toughness (iFT) approach at the 2009 Academy of Dental Materials meeting (Portland, OR), the technical complexity of fracture toughness testing probably discouraged researchers from producing new fracture toughness data. Triggered by this symposium, we first developed a macro-iFT test (De Munck et al. 2013; De Munck et al. 2015). Here, we introduced a miniiFT version, which appeared almost as feasible as common microtensile bond strength testing; it caused specimens to fail at the actual interface with lower variation (Pongprueksa et al. 2016). We therefore encourage other researchers to pick up this novel approach. Meanwhile, further validation was conducted in the framework of the PhD thesis of Dr. Pongprueksa (2016). Bonding effectiveness can be measured in different ways— in this case, through common bond strength testing but also through an iFT approach. We use bonding effectiveness as a compilation term for the perceived effectiveness of an adhesive to bond. Acknowledgments