Does the universal adhesive's film thickness affect dentin-bonding effectiveness?

OBJECTIVES: To investigate the influence of adhesive resin application modalities on the film thickness of the adhesive resin and the effectiveness of a two-step universal adhesive (UA) bonded in self-etch (SE) bonding mode to high C-factor class-I cavity-bottom dentin. MATERIALS AND METHODS: After application of the primer of G2-Bond Universal (G2B, GC), the adhesive resin was applied into standard class-I cavities (human molars) following four application modalities: (1) one layer, strongly air-blown; (2) one layer, gently air-blown; (3) two layers, each gently air-blown; (4) one layer, not air-blown. After being restored with composite, each tooth was sectioned to obtain one micro-specimen (n = 10), of which the adhesive resin film thickness was measured using optical microscopy. The micro-tensile bond strength (µTBS) was tested immediately or upon 100,000 thermocycles. Statistical analyses involved Kruskal-Wallis and Mann-Whitney U testing (p < 0.05). RESULTS: G2B's µTBS was significantly affected by the adhesive resin application modality and aging. Gently air-blowing the adhesive resin resulted in significantly higher immediate µTBS than strong air-blowing or no air-blowing. No significant difference in µTBS was found between single or double gently air-blown adhesive resin applications. The adhesive resin film thickness significantly varied with the application modalities. CONCLUSIONS: A too thin or too thick adhesive resin film thickness adversely affected bond strength of the two-step UA applied in SE mode and high C-factor condition. CLINICAL RELEVANCE: The adhesive resin layer thickness can affect the bonding performance of two-step UAs in high C-factor cavities. Dental clinicians remain advised to avoid improper air-blowing of UAs and strictly follow the application instructions.

Bonding of Composite Cements Containing 10-MDP to Zirconia Ceramics Without Dedicated Ceramic Primer.

PURPOSE: To measure zirconia-to-zirconia microtensile bond strength (µTBS) using composite cements with and without primer. MATERIALS AND METHODS: Two Initial Zirconia UHT (GC) sticks (1.8x1.8x5.0 mm) were bonded using four cements with and without their respective manufacturer's primer/adhesive (G-CEM ONE [GOne] and G-Multi Primer, GC; Panavia V5 [Pv5]), and Panavia SA Cement Universal [PSAu], and Clearfil Ceramic Plus, Kuraray Noritake; RelyX Universal (RXu) and Scotchbond Universal Plus [SBUp], 3M Oral Care). Specimens were trimmed to an hour-glass shaped specimen whose isthmus is circular in cross-section. After 1-week water storage, the specimens were either tested immediately (1-week µTBS) or first subjected to 50,000 thermocycles (50kTC-aged µTBS). The fracture mode was categorized as either adhesive interfacial failure, cohesive failure in composite cement, or mixed failure, followed by SEM fracture analysis of selected specimens. Data were analyzed using linear mixed-effects statistics (α = 0.05; variables: composite cement, primer/adhesive application, aging). RESULTS: The statistical analysis revealed no significant differences with aging (p = 0.3662). No significant difference in µTBS with/without primer and aging was recorded for GOne and PSAu. A significantly higher µTBS was recorded for Pv5 and RXu when applied with their respective primer/adhesive. Comparing the four composite cements when they were applied in the manner that resulted in their best performance, a significant difference in 50kTC-aged µTBS was found for PSAu compared to Pv5 and RXu. A significant decrease in µTBS upon 50kTC aging was only recorded for RXu in combination with SBUp. CONCLUSION: Adequate bonding to zirconia requires the functional monomer 10-MDP either contained in the composite cement, in which case a separate 10-MDP primer is no longer needed, or in the separately applied primer/adhesive.

Experimental two-step universal adhesives bond durably in a challenging high C-factor cavity model.

OBJECTIVES: To determine the bonding effectiveness of experimental 2-step universal adhesives (UAs) to high C-factor class-I cavity-bottom dentin and to assess the potential bond-strength contribution of an additional flowable composite layer. METHODS: Three experimental 2-step UA formulations, involving the application of a 10-MDP-based primer followed by a hydrophobic adhesive resin with a 15-to-20-µm film thickness and differing only for filler, referred to as BZF-21 (silica and bioglass filler), BZF-29 (silica filler) and BZF-29_hv (higher silica-filler loading resulting in a higher viscosity), all prepared by GC, along with three representative commercial adhesives, Clearfil SE Bond 2 (C-SE2, Kuraray Noritake), G-Premio Bond (G-PrB, GC) and OptiBond FL (Opti-FL, Kerr), were comparatively investigated for their 'immediate' and 'aged' (50,000 thermocycles) micro-tensile bond strength (µTBS), when applied either in etch-and-rinse (E&R) or self-etch (SE) mode, to high C-factor class-I cavity-bottom dentin (n = 10; 10 experimental groups). Four additional experimental groups involved the extra application of the flowable composite G-ænial Universal Flo (GC), employed as an intermediate liner in combination with the adhesives BZF-29 and G-PrB and again applied both in E&R or SE mode. Statistical analysis was performed using linear mixed-effects (LME) modelling and linear regression analysis (p < 0.05). RESULTS: All 2-step UAs performed similarly when compared to the gold-standard E&R Opti-FL and SE C-SE2 adhesives, except for the aged µTBS of BZF-29_hv applied in E&R mode, and significantly outperformed the 1-step UA G-PrB. Significant reduction in µTBS upon aging was only recorded for 2-step UAs applied in E&R mode. The extra flowable composite layer significantly improved G-PrB's µTBS. SIGNIFICANCE: The experimental 2-step UAs revealed favorable bonding performance in the challenging high C-factor class-I cavity model, comparable to that of the multi-step gold-standard E&R and SE adhesives and superior to that of the 1-step UA investigated. An additionally applied flowable composite layer compensated for the lower bonding effectiveness of the 1-step UA in the high C-factor cavity model.

Adhesive Performance Assessment of Universal Adhesives and Universal Adhesive/Composite Cement Combinations.

PURPOSE: To investigate the bonding performance of three universal adhesives (UAs) to dentin and the effect of different curing modes and hydrofluoric-acid (HF) etching of lithium-disilicate glass-ceramic on the adhesive performance of two UA/composite cement (CC) combinations. MATERIALS AND METHODS: In the first project part, the immediate and aged (25k and 50k thermocycles) microtensile bond strength (µTBS) of the two light-curing UAs G2-Bond Universal (G2B; GC) and Scotchbond Universal Plus (SBUp; 3M Oral Care), and the self-curing UA Tokuyama Universal Bond II (TUBII; Tokuyama) to flat dentin was measured, when applied in both E&R and SE bonding mode using a split-tooth design (n = 10). The resultant adhesive-dentin interfaces were characterized using TEM. In the second project part, CAD/CAM composite blocks were luted to flat dentin with either Scotchbond Universal Plus/RelyX Universal (SBUp/RxU; 3M Oral Care) or Tokuyama Universal Bond II/Estecem II Plus (TUBII/ECIIp; Tokuyama Dental) using different curing modes (AA mode: auto-curing of both adhesive and cement; AL mode: auto-curing of adhesive and light-curing of cement), upon which their immediate and aged (25k and 50k thermocycles) µTBS was measured. In the third project part, the same UA/CC combinations were luted to CAD/CAM glass-ceramic to measure their immediate and aged (6-month water storage) shear bond strength (SBS). RESULTS: In E&R bonding mode, the performance of G2B, SBUp and TUBII was not significantly different in terms of µTBS, while G2B and SBUp significantly outperformed TUBII in SE bonding mode. No significant difference in µTBS was found between the SBUp/RxU and TUBII/ECIIp UA/CC combinations, regardless of bonding mode, aging time, or curing mode. The cement-curing mode did not significantly influence µTBS, while a significantly higher µTBS was recorded for the UA/CC combinations applied in E&R bonding mode. HF significantly improved the SBS of the UA/CC combinations to glass-ceramic. CONCLUSION: The self-curing adhesive performed better when applied in E&R than in SE bonding mode. The curing mode did not influence the adhesive performance of the composite cements, while an E&R bonding mode rendered more favorable adhesion in a self-curing luting protocol. When bonding to glass-ceramic, the adhesive performance of the universal adhesive/composite cement combinations benefited from HF etching.

Mini-iFT Confirms Superior Adhesive Luting Performance using Light-curing Restorative Composites.

PURPOSE: To validate the rationale of using a conventional light-curing resin-based composite (RBC) to lute thick indirect restorations by measuring mini-interfacial fracture toughness (mini-iFT). MATERIALS AND METHODS: Freshly exposed dentin of extracted third molars (n = 64) was immediately sealed with a thin layer of an experimental RBC with a 50 wt% or 75 wt% (IDS) filler load. Two- or 6-mm-thick CAD/CAM composite blocks were luted onto IDS using either pre-heated light-cure or dual-cure luting RBC, with the latter having served as control. Samples were cut into sticks, upon which a notch was prepared at the interface between IDS and luting RBC, prior to being submitted to a 4-point bending test to determine mini-iFT. The results were analyzed using a mixed linear model (LME). Failure mode at the fractured interface was determined using scanning electron microscopy (SEM). RESULTS: LME revealed that mini-iFT was not significantly affected by the composite block thickness (p = 0.39), but by the luting RBC (p < 0.0001) and the IDS RBC filler load (p = 0.0011). Mini-iFT was higher with 50 wt% filler-loaded RBC IDS and when luted using the light-curing RBC. CONCLUSION: This work provides the proof of concept that 2- and 6-mm-thick indirect restorations can safely be adhesively luted with pre-heated conventional light-cure RBC under controlled light-irradiation conditions. This strategy even seems beneficial in terms of mini-iFT compared to using a dual-cure luting RBC. IDS with lower filler content also appeared more favorable.

Optimizing glass-ceramic bonding incorporating new silane technology in an experimental universal adhesive formulation.

OBJECTIVE: Incorporating silane-coupling agent into universal adhesives (UAs) to simplify adhesive luting of glass-ceramic restorations appeared ineffective due to silane's instability in an acidic aqueous solution. This study aimed to evaluate new silane technology added to an experimental UA to be bonded to glass ceramics without separate prior silanization. METHODS: Combined silane technology, consisting of 3-(aminopropyl)triethoxysilane (APTES) and γ-methacryloxypropyltriethoxysilane (γMPTES), was incorporated into an experimental UA formulation, being referred to as ADH-XTE (3M Oral Care). Immediate and aged shear bond strength (SBS) of ADH-XTE onto as-milled ('AM'), tribochemical silica-coated ('TSC'), HF-etched ('HF'), and mirror-polished ('MP') glass-ceramic CAD/CAM blocks (IPS e.max CAD) with/without separate silanization was measured (n = 10/group). The control adhesives included Scotchbond Universal ('SBU') and Scotchbond 1 XT ('SB1-XT'). The glass-ceramic surface topography and the fractography of the SBS-debonded specimens were observed by SEM. RESULTS: Without separate prior silanization, the experimental UA ADH-XTE, containing combined APTES/γMPTES silane technology, significantly outperformed the glass-ceramic bonding efficiency of its silane-containing SBU precursor, while it performed equally effective as SBU applied with prior silanization. Upon aging, significant reduction in SBS was recorded when ADH-XTE was bonded to TSC glass-ceramic surfaces (p < 0.05), while not to HF ones. Notably, the lowest SBS was obtained when the UAs were bonded to AM and MP glass-ceramic surfaces, in particular when applied without separate prior silanization (p < 0.05). SIGNIFICANCE: The glass-ceramic bonding capacity of the new combined APTES/γMPTES silane-containing UA ADH-XTE surpassed that of its SBU precursor. HF etching remains needed to durably bond to glass-ceramics.

Structural/Chemical Characterization and Bond Strength of a New Self-Adhesive Bulk-fill Restorative.

PURPOSE: The material structure and chemical elemental composition of a new self-adhesive composite hybrid were investigated. The bonding performance when applied on flat (FLAT) vs high C-factor class-I cavity-bottom (CAVITY) dentin and in light-cure (LC) vs self-cure (SC) mode was determined. MATERIALS AND METHODS: The self-adhesive bulk-fill composite Surefil One (Su-O; Dentsply Sirona) was compared with the resin-modified glass-ionomer Fuji II LC Improved (Fuji2LC; GC) and the ion-releasing alkasite material Cention N (CentionN; Ivoclar Vivadent). The material structure was examined with SEM and TEM, while the chemical elemental composition was analyzed using EDS. The immediate and aged microtensile bond strength (µTBS) of Su-O_LC/SC was compared to that of Fuji2LC applied without any pre-treatment, and to that of CentionN applied following bonding with Adhese Universal (AU) (Ivoclar Vivadent) in self-etch mode (AU/CentionN). All restorative materials were bonded onto FLAT and CAVITY dentin. Statistical analysis was performed with the Kruskal-Wallis nonparametric test. RESULTS: EDS analysis revealed that Su-O was richer in C and P than the reference restorative materials. Applied to FLAT dentin, the significantly highest immediate and aged µTBS were recorded for AU/CentionN, which were not significantly different only from Su-O_LC. Applied to CAVITY dentin, the significantly highest immediate µTBS was recorded for AU/CentionN, which did not differ significantly only from Su-O_SC. Su-O_LC bonded to CAVITY dentin suffered from a high incidence of pre-test failures. CONCLUSION: While Su-O_LC bonded effectively and durably to FLAT dentin, Su-O_SC bonded more favorably than Su-O_LC in class-I cavities, which was probably related to shrinkage stress variously challenging the respective bond.

Zinc-Calcium-Fluoride Bioglass-Based Innovative Multifunctional Dental Adhesive with Thick Adhesive Resin Film Thickness.

Apart from producing high bond strength to tooth enamel and dentin, a dental adhesive with biotherapeutic potential is clinically desirable, aiming to further improve tooth restoration longevity. In this laboratory study, an experimental two-step universal adhesive, referred to as Exp_2UA, applicable in both the etch-and-rinse (E&R) and self-etch (SE) modes and combining a primer, containing 10-methacryloyloxydecyldihydrogen phosphate as a functional monomer with chemical binding potential to hydroxyapatite, with a bioglass-containing hydrophobic adhesive resin, was multifactorially investigated. In addition to primary property assessment, including measurement of bond strength, water sorption, solubility, and polymerization efficiency, the resultant adhesive-dentin interface was characterized by transmission electron microscopy (TEM), the filler composition was analyzed by energy-dispersive X-ray spectroscopy, and the bioactive potential of the adhesive was estimated by measuring the long-term ion release and assessing its antienzymatic and antibacterial potential. Four representative commercial adhesives were used as reference/controls. Application in both the E&R and SE modes resulted in a durable bonding performance to dentin, as evidenced by favorable 1 year aged bond strength data and a tight interfacial ultrastructure that, as examined by TEM, remained ultramorphologically unaltered upon 1 year of water storage aging. TEM revealed a 20 µm thick hydrophobic adhesive layer with a homogeneous bioglass filler distribution. Adequate polymerization conversion resulted in extremely low water sorption and solubility. In situ zymography revealed reduced endogenous proteolytic activity, while Streptococcus mutans biofilm formation was inhibited. In conclusion, the three-/two-step E&R/SE Exp_2UA combines the high bonding potential and bond degradation resistance with long-term ion release, rendering the adhesive antienzymatic and antibacterial potential.

Bonding to enamel using alternative Enamel Conditioner/etchants.

OBJECTIVE: Enamel bond durability of three new alternative etchants combined with three representative adhesives was determined. METHODS: The 'immediate' and 'aged' micro-tensile bond strength (µTBS) of the 3-step etch&rinse adhesive OptiBond FL ('O-FL', Kerr), 2-step self-etch (SE) adhesive Clearfil SE Bond 2 ('C-SE2', Kuraray Noritake) and universal adhesive Adhese Universal ('ADU', Ivoclar Vivadent) were measured when bonded to enamel following either a proprietary organic acid-containing Enamel Conditioner ('EC', Shofu), a phosphoric-acid monomer-containing Multi Etchant ('ME', Yamakin: 10-methacryloyloxy tetraethylene glycol dihydrogenphosphate or MTEGP), or a metal salt-based ZON etchant ('ZON', Ivoclar Vivadent: ZrO(NO3)2). All alternative etchants were used in replacement of phosphoric acid, the latter (K-Etchant, Kuraray Noritake) also used with O-FL and ADU, in addition to C-SE2 that was solely used in SE mode (controls). The enamel-etching patterns and de-bonded fracture surfaces were examined by SEM, while the interfaces with enamel were ultra-morphologically characterized by TEM. RESULTS: No statistically significant difference in immediate and aged µTBS, obtained by combining the three alternative etchants with the three adhesives, was recorded as compared with the respective controls, except for ME combined with O-FL. Upon aging, significant reduction in µTBS was recorded for the ME/C-SE2 and ME/ADU combinations. The percentage of adhesive failures increased with aging. SEM revealed similar etching patterns produced by EC and ZON as by classic phosphoric-acid etching, for which also numerous micro-resin tags at the adhesive-enamel interface were disclosed. SIGNIFICANCE: Durable bonding to enamel was generally obtained for all etchant/adhesive combinations with the exception of the ME/O-FL combination.