Hydroxyapatite effect on photopolymerization of self-etching adhesives with different aggressiveness

Objective

To understand the correlation of the acidic monomer/hydroxyapatite (HAp) reaction with the photopolymerization behaviour of self-etching adhesives with different aggressiveness.

Methods

Two commercial self-etching adhesives the strong Adper Prompt L-Pop (APLP, pH ∼ 0.8) and the mild Adper Easy Bond (AEB, pH ∼ 2.5) were used. HAp powders were incorporated into both adhesives to acquire solutions with concentrations of 0, 1, 3, 5, 7 wt%. The attenuated total reflectance Fourier transform infrared (ATR/FT-IR) technique was employed to collect the in situ spectra during light-curing, from which the degree of conversion (DC) and polymerization rate (PR) were calculated. The pH of each tested solution was also measured.

Results

Without HAp incorporation, the DC and PR of the strong APLP (7.8% and 0.12%/s, respectively) were much lower than those of the mild AEB (85.5% and 5.7%/s, respectively). The DC and PR of APLP displayed an apparent increasing trend with the HAp content. For example, the DC increased from 7.8% to 58.4% and the PR increased from 0.12 to 3.8%/s when the HAp content increased from 0 to 7 wt%. In contrast, the DC and PR of AEB were much less affected by the HAp content. The observations were correlated well with the spectral and pH changes, which indicated that APLP underwent a higher extent of chemical reaction with HAp than AEB.

Conclusions

The results disclosed the important role of the acidic monomer/HAp chemical reaction in improving the photopolymerization of the strong (low-pH) self-etching adhesives such as APLP. The phenomenon of polymerization improvement strongly depended on the adhesive aggressiveness.     

Effect of application mode on interfacial morphology and chemistry between dentine and self-etch adhesives

Objective

To investigate the influence of application mode on the interfacial morphology and chemistry between dentine and self-etch adhesives with different aggressiveness.

Methods

The occlusal one-third of the crown was removed from un-erupted human third molars, followed by abrading with 600 grit SiC under water. Rectangular dentine slabs were prepared by sectioning the tooth specimens perpendicular to the abraded surfaces. The obtained dentine slabs were treated with one of the two one-step self-etch adhesives: Adper Easy Bond (AEB, pH ∼ 2.5) and Adper Prompt L-Pop (APLP, pH ∼ 0.8) with (15 s, active application) or without (15 s, inactive application) agitation. The dentine slabs were fractured and the exposed adhesive/dentine (A/D) interfaces were examined with micro-Raman spectroscopy and scanning electron microscopy (SEM).

Results

The interfacial morphology, degree of dentine demineralization (DD) and degree of conversion (DC) of the strong self-etch adhesive APLP showed more significant dependence on the application mode than the mild AEB. APLP exhibited inferior bonding at the A/D interface if applied without agitation, evidenced by debonding from the dentine substrate. The DDs and DCs of the APLP with agitation were higher than those of without agitation in the interface, in contrast to the comparable DD and DC values of two AEB specimen groups with different application modes. Raman spectral analysis revealed the important role of chemical interaction between acid monomers of self-etch adhesives and dentine in the above observations.

Conclusion

The chemical interaction with dentine is especially important for improving the DC of the strong self-etching adhesive at the A/D interface. Agitation could benefit polymerization efficacy of the strong self-etch adhesive through enhancing the chemical interaction with tooth substrate.     

Monomer-to-polymer conversion and micro-tensile bond strength to dentine of experimental and commercial adhesives containing diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide or a camphorquinone/amine photo-initiator system

Objectives

To compare the degree of conversion (DC) of adhesives initiated by diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide (TPO) or a camphorquinone/tertiary amine system (CQ/Amine) as well as their ‘immediate’ micro-tensile bond strength (μTBS) to bur-cut dentine.

Methods

DC of Scotchbond Universal (‘SBU’; 3M ESPE), its experimental counterpart containing TPO as photo-initiator system, an experimental G-aenial Bond (‘Ga-B’; GC) adhesive formulation, and an experimental LUB-102 adhesive formulation (‘LUB’, Kuraray Noritake), containing as photo-initiatior system either 2 wt% CQ along with 2 wt% tertiary amine (‘SBU_CQ/Amine’; ‘Ga-B_CQ/Amine’; ‘LUB_CQ/Amine’), or 2 wt% TPO (‘SBU_TPO’; ‘Ga-B_TPO’; ‘LUB_TPO’), was determined using Fourier-transform infrared spectroscopy (FTIR), after being cured with a dual-wavelength light-curing unit (bluephase 20i, Ivoclar Vivadent). The same adhesive formulations were applied to bur-cut mid-coronal dentine of intact human molars, and subjected to a μTBS test after 1-week water storage. Besides being applied following a self-etch (SE) application mode, the adhesive formulations SBU_CQ/Amine and SBU_TPO were also applied following an etch-and-rinse (E&R) mode, this both for DS and μTBS measurement.

Results

No significant difference in DC was found for any of the adhesive formulations, except for SBU_CQ/Amine_SE and SBU_TPO_SE. For both SBU formulations, a significantly higher DC was reached for the E&R than the SE approach. Regarding μTBS, no significant differences were recorded, except for the significantly higher μTBS measured for SBU_CQ/Amine_E&R and SBU_TPO_E&R.

Conclusions

In self-etch adhesives, the photo-initiator TPO may be used instead of CQ/Amine. The curing and ‘immediate’ bonding efficiency depended on the application protocol (E&R versus SE), but not on the photo-initiator system.

Clinical significance

The photo-initiator TPO may be used in self-etch adhesives instead of CQ/Amine with similar curing and ‘immediate’ bonding efficiency.     

Effect of natural cross-linkers incorporation in a self-etching primer on dentine bond strength

Objectives

The aim of this in vitro study was to investigate the effect of incorporation of natural cross-linkers into the primer of a self-etching adhesive on resin–dentine bond strength.

Methods

Flat dentine surfaces were prepared from extracted human molar teeth and were applied with the following self-etching primers. The 0.5% hesperidin (HPN), 0.5% chlorhexidine (CHX) or 0.5% grape seed extract (GSE) was incorporated into Clearfil SE primer (Kuraray Medical, Inc.) to formulate three experimental primers. The original SE primer served as control. Following primer application, the teeth were bonded with Clearfil SE bond, restored with resin composite and stored in water for 24 h at 37 °C. The bonded specimens were sectioned into beams and subjected to micro tensile bond testing (μTBS). Failure analysis and morphological evaluation of the dentine surfaces were performed using a scanning electron microscope (SEM). Hardness (H) and elastic modulus (EM) were measured using nano-indentation technique to examine the mechanical properties of the bonded interfaces.

Results

One-way ANOVA showed significant differences in μTBS, H and EM among the tested and control groups (p < 0.001). Tukey post hoc test revealed that incorporation of HPN significantly increased μTBS, H and EM, when compared with the other groups (p < 0.006). The GSE-incorporated group significantly decreased μTBS, H and EM, when compared with the other groups (p < 0.006); while CHX-incorporated group did not show any statistical significant difference when compared with the control group.

Conclusion

Incorporation of HPN into Clearfil SE primer had a positive influence on the immediate μTBS and mechanical properties of the bonded interface.     

pH changes of self-etching primers mixed with powdered dentine

OBJECTIVES: The purpose of this study was to examine the pH changes of self-etching primers mixed with dentine powder. METHODS: Four self-etching primer adhesive systems were used: Clearfil SE Bond, Imperva Fluoro Bond, Mac Bond II, and Unifil Bond. Dentine discs obtained from extracted bovine incisors were milled and pulverized into a fine powder. The dentine powder was then mixed with solutions of self-etching primers diluted with distilled water. The pH changes of the primer-dentine powder mixtures were measured by a solid-state pH sensor connected to a pH meter at time points 10, 20, 30, 60, 120, 180, 300, and 600 s after the start of mixing. Data were analyzed by the Tukey HSD test and the Dunnett test at a significance level of 0.05. RESULTS: The baseline pH values of the self-etching primers ranged from 1.83 to 2.34, with Mac Bond II exhibiting a significantly lower value than the other three products. After mixing with the dentine powder, the pH values significantly increased, ranging from 6.95 to 7.37 at 600 s after mixing; there were no significant differences in these values among the self-etching primers used. An insoluble precipitate was formed in the case of Clearfil SE Bond, indicating a chemical reaction between the functional monomer and the dentine powder. CONCLUSIONS: The dentine has a strong buffering capacity against the acidity of self-etching primers.     

Modifications of the organic and mineral fractions of dental tissues following conditioning by self-etching adhesives

Objectives

Our objective was to analyse the acid strengths and concentrations in contemporary self-etch adhesives and test whether the adhesion/decalcification concept functions the same way for all products.

Methods

The self-etching adhesives were dissolved in a 50% water-ethanol solvent, these were reacted with biological apatite (HA) in the form of powder of human dentine in order to quantify calcium release and study the reaction products as a function of acid strengths and concentrations. The four self-etching adhesives investigated were AdheSE One (Ivoclar Vivadent, Schaan, Liechtenstein), Adper Easy Bond (3 M ESPE, St Paul, MN, USA), Optibond All-In-One (KERR, Orange, CA, USA), Xeno V (Dentsply De Trey, Konstanz, Germany).

Results

Acid concentrations were found to span the range from 1 to 2 mmol/l, and the acid dissociation constants varied between apparent pKa values of 3.4 and 4.2. The pH values changed with time from values near 2.8 to 3.6, confirming the buffering action of HA. The stronger acids dissolved more calcium ions but left less organic matter attached to the tissue particles. Thermogravimetric and infrared analysis demonstrated that the weaker acids tended to bind to HA surfaces and increased significantly the organic to mineral ratios of the powders.

Conclusion

Self-etching adhesives can be differentiated and classified in two types: weak acids attach to the mineral phase and leach little calcium; strong acids bind to the calcium ions, demineralize more and tend to debond from the dentinal hard tissues by forming more soluble calcium salts.     

Nd：YAG激光对自酸蚀粘结系统和牙本质粘结力的影响

目的探讨Nd：YAG激光对牙本质自酸蚀粘结系统的影响。方法选用因正畸拔除的新鲜前磨牙42颗，随机分为3组，每组14颗；牙面预备暴露牙本质；分别采用Adper^TM Prompt^TM粘结剂＋F2000树脂充填，Nd：YAG激光照射＋Adper^TM Prompt^TM粘结剂＋F2000树脂充填，Adper^TM Prompt^TM粘结剂＋Nd：YAG激光照射＋F2000树脂充填。评价各组树脂与牙本质之间剪切强度。结果Nd：YAG激光照射＋Adper^TM Prompt^TM粘结剂＋F2000树脂充填组的剪切强度明显大于其余2组，其余2组之间剪切强度对比无明显差异。结论先采用脉冲Nd：YAG激光照射后使用Adper^TM Prompt^TM粘结剂组获得最大粘结力。     

Long-term follow-up of composite resin restorations with self-etching adhesives

OBJECTIVE: To test the hypothesis, derived from a previous short-term (7-day) assessment, that the absence of conventional pulp protection is not responsible for long-term pulp complications of composite resin restorations with self-etching adhesives. METHODS: All 150 patients who received the restorations with self-etching adhesives were recalled at least 2 years after the placement of restorations. Of the 47 patients (31%) who responded, 106 restorations aged from 2.2 to 6.5 years were examined for tooth sensitivity and pulp vitality regarding long-term pulp complications. The results were subjected to a multivariable logistic regression analysis with regard to cavity depth, provision of conventional pulp protection and short-term pulp complications. RESULTS: No positive cases were found in the assessment of tooth sensitivity. Four restorations (3.7%) made in deep cavities with conventional pulp protection resulted in pulpectomy due to inflammation, of which three cases presented short-term pulp complications. The 95% confidence intervals for the odds ratios estimated by the multivariable logistic regression analysis were (1.54, infinity) for cavity depth (1.50, infinity) for short-term pulp complications and (0.02, infinity) for conventional pulp protection. Namely, the last variable had no significant effect on long-term pulp complications and thus the hypothesis was verified. CONCLUSIONS: The absence of conventional pulp protection was not responsible for long-term pulp complications even in deep cavities with the use of self-etching adhesives. A deep cavity and the existence of short-term pulp complications were two critical predictors for the occurrence of long-term pulp complications.     

Quantitative micro-Raman assessment of dentine demineralization, adhesive penetration, and degree of conversion of three dentine bonding systems

Unreacted monomers in adhesive systems may cause a reduction in material properties, an increase in the long-term instability of the restoration, and pulpal irritation. The degree of dentine demineralization, adhesive penetration, and the degree of conversion (DC) across the dentine–adhesive interface of self-etch adhesives were measured using micro-Raman spectroscopy. Two-step, self-etch AdheSE, one-step self-etch AdheSE One, and etch-and-rinse Excite (control) (Ivoclar Vivadent AG, Schaan, Liechtenstein) were studied. Nine human molars were allocated to three groups and a flat dentine surface was prepared. A smear layer was produced by grinding dentine with 600-grit silicone-carbide discs under water. After application and polymerization of the adhesive, teeth were sectioned to produce four 1–mm-thick slices per tooth for micro-Raman spectroscopy. There were statistically significant differences in the depth of dentine demineralization between all adhesives. The depth and degree of demineralization decreased in the order: Excite>AdheSE>AdheSE One. The mean ± standard deviation (SD) values for DC within the adhesive layer were 85.2 ± 2.9% (Excite), 81.4 ± 4.2% (AdheSE), and 54.3 ± 10.1% (AdheSE One), and within the hybrid layer were 55.2 ± 22.5% (Excite), 65.1 ± 16.9% (AdheSE), and 42.0 ± 16.2% (AdheSE One). All systems showed a discrepancy between dentine demineralization and adhesive penetration. A significant amount of unreacted monomers were associated with all systems but particularly with the etch-and-rinse system.     

Immediate bonding properties of universal adhesives to dentine

ObjectivesTo evaluate the dentine microtensile bond strength (μTBS), nanoleakage (NL), degree of conversion (DC) within the hybrid layer for etch-and-rinse and self-etch strategies of universal simplified adhesive systems.Methodsforty caries free extracted third molars were divided into 8 groups for μTBS (n = 5), according to the adhesive and etching strategy: Clearfil SE Bond [CSE] and Adper Single Bond 2 [SB], as controls; Peak Universal Adhesive System, self-etch [PkSe] and etch-and-rinse [PkEr]; Scotchbond Universal Adhesive, self-etch [ScSe] and etch-and-rinse [ScEr]; All Bond Universal, self-etch [AlSe] and etch-and-rinse [AlEr]. After restorations were constructed, specimens were stored in water (37 °C/24 h) and then resin–dentine sticks were prepared (0.8 mm²). The sticks were tested under tension at 0.5 mm/min. Some sticks from each tooth group were used for DC determination by micro-Raman spectroscopy or nanoleakage evaluation (NL). The pH for each solution was evaluated using a pH metre. Data were analyzed with one-way ANOVA and Tukey's test (α = 0.05).ResultsFor μTBS, only PkSe and PkEr were similar to the respective control groups (p > 0.05). AlSe showed the lowest μTBS mean (p < 0.05). For NL, ScEr, ScSe, AlSe, and AlEr showed the lowest NL similar to control groups (p < 0.05). For DC, only ScSe showed lower DC than the other materials (p < 0.05).ConclusionsPerformance of universal adhesives was shown to be material-dependent. The results indicate that this new category of universal adhesives used on dentine as either etch-and-rinse or self-etch strategies were inferior as regards at least one of the properties evaluated (μTBS, NL and DC) in comparison with the control adhesives (CSE for self-etch and SB for etch-and-rinse).     

The effect of excitation laser power in Raman spectroscopic measurements of the degree of conversion of resin composites

ObjectivesTo evaluate the effect of excitation laser power in Raman spectrometry by comparing the spectra and the degree of conversion (DC) values obtained using excitation powers between 300 and 1000 mW.MethodsFive commercial and three experimental resin composites were light cured at 1200 mW/cm² for 10–20 s from a commercial blue-violet LED dental curing unit. Raman spectra were collected from composite specimens within 9 min after light-curing. The excitation laser (1064 nm) was focused on the spot of 0.4 mm in diameter. The following powers were used for specimen excitation (mW): 300, 400, 600, 800, and 1000. From Raman spectra, the DC values were calculated and compared among different laser powers. Also, vector-normalized Raman spectra collected using the lowest excitation power (300 mW) were compared to those collected using the maximum excitation power (1000 mW).ResultsVarying the excitation laser power between 300 and 1000 mW resulted in statistically significant differences in both the DC values and the intensity of particular spectral features. The effect of varying laser power on Raman spectra and obtained DC values was material-dependent. The DC values measured within an individual material using different laser powers varied between 3.2 and 7.2% (absolute DC difference). The spectral bands affected by variations in laser power were assigned to symmetric and asymmetric stretching of −CH₂ (2900-3100 cm⁻¹), symmetric stretching of aliphatic CC (1640 cm⁻¹) and scissoring of C–H (1458 cm⁻¹).SignificanceThe DC can be artificially elevated through increasing excitation laser power. This effect should be considered in Raman spectroscopic evaluations of DC in specimens during ongoing post-cure polymerization.     

Influence of the degree of dentine mineralization on pulp chamber temperature increase during resin-based composite (RBC) light-activation

Objectives

To analyse the influence of the degree of dentine mineralization on the pulp chamber temperature increase during composite light-activation.

Methods

Dentine discs (2 mm thick) obtained from recently extracted teeth or those with extensive dentine sclerosis were analysed by FT-IR spectrometry in order to choose the two discs with the greatest difference in the degree of mineralization. A model tooth was set up with the dentine discs between a molar with the pulp chamber exposed and a crown with a standardized class II cavity. A K-type thermocouple was introduced into the molar root until it came into contact with the dentine discs and the cavity was filled with P60 resin composite. The temperature rise was measured for 120 s after light-activation began: Standard (S) 600 mW/cm²/40 s; Ramp (R) 0 → 800 mW/cm²/10 s + 800 mW/cm²/10 s; Boost (B) 850 mW/cm²/10 s and LED (L) 1.300 mW/cm²/40 s (n = 10). The same protocol was repeated after grinding the dentine discs to 1.0 and 0.5 mm thickness.

Results

The temperature increase was significantly higher in dentine with high degree of mineralization (p < 0.05). With respect to the dentine thickness, the following result was found: 2 mm < 1 mm < 0.5 mm (p < 0.05). The light-activation mode also presented significant difference as follows: S > R = L > B (p < 0.05).

Conclusions

The higher the degree of dentine mineralization the greater the increase in pulp chamber temperature. The temperature increase was influenced by the light-polymerization mode and dentine thickness.     

Relationship between contraction stress and degree of conversion in restorative composites

OBJECTIVES: To verify the relationship between contraction stress and degree of conversion (DC) in different composites (Filtek Z250, Filtek A110, Tetric Ceram and Heliomolar). METHODS: For the contraction stress test, composite (2 mm thick) was applied between two 5-mm diameter glass rods, mounted in a tensilometer. DC was determined by Infrared Photoacoustic spectroscopy in specimens with similar dimensions and geometry, submitted to identical curing conditions. Specimens were exposed to different energy densities (4.5, 13.5, 27.0, 54.0 and 108.0 J/cm2) by varying exposure time. Contraction stress and DC were recorded 10 min after the beginning of photoactivation. Results were analyzed by ANOVA/Tukey's test and regression analysis. RESULTS: For contraction stress, the interaction between composite and energy density was significant. Stress values ranged between 0.6+/-0.2 and 2.0+/-0.3 MPa at 4.5 J/cm2, 2.3+/-0.5 and 4.3+/-0.4 MPa at 13.5 J/cm2, 3.8+/-0.5 and 5.8+/-0.9 MPa at 27.0 J/cm2, 4.2+/-0.8 and 7.9+/-0.9 MPa at 54.0 J/cm2 and 6.6+/-0.8 and 8.1+/-0.9 MPa at 108.0 J/cm2. Tetric Ceram (39+/-5.8%) showed a higher average DC than the other materials. Heliomolar (28+/-5.2%) showed an average DC similar to Filtek Z250 (32+/-6.6%) and to Filtek A110 (24+/-7.5%) regardless of the energy density level. No significant increase in DC was observed above 27 J/cm2. CONCLUSIONS: At high energy levels, DC had a tendency to level off earlier than contraction stress values. SIGNIFICANCE: Using high energy densities may cause a significant increase in stress values, without producing a significant increase in conversion.     

原花青素预处理对全酸蚀粘接系统双键转化率的影响

将葡萄籽提取物原花青素(proanthocyanidin,PA)分别用乙醇、丙酮、蒸馏水配制成不同浓度的预处理剂,利用傅里叶红外光谱测试PA预处理对Single Bond 2和Prime＆Bond NT两种全酸蚀粘接系统双键转化率的影响.结果发现不同溶剂、浓度的PA预处理剂组2种全酸蚀粘接剂的双键转化率与阴性对照组均无统计学差异(P＞0.05).提示原花青素预处理对全酸蚀粘接系统固化性能无显著影响.     

The role of spacer carbon chain in acidic functional monomers on the physicochemical properties of self-etch dental adhesives

Objectives

To evaluate the effects of acidic functional monomers with different hydrophilicity and spacer carbon chain length on the degree of conversion (DC), wettability (contact angle), water sorption (WS) and ultimate tensile strength (UTS) of experimental one-step self-etch adhesives (1-SEAs).

Methods

A series of standard resin blends was prepared with each formulation containing 15 mol% of each acidic monomer. The structural variations of the acidic monomers were MEP (spacer chain with 2 carbons), MDP (10-carbons), MDDP (12-carbons), MTEP (more hydrophilic polyether spacer) and CAP-P (intermediate hydrophilicity ester spacer). Dumbbell-shaped and disc specimens were prepared and tested for UTS and WS, respectively. DC was assessed by FTIR, while the wettability of each 1-SEA was evaluated on glass slides and flat dentine surfaces. Results were analysed with one-way ANOVA and Tukey's test (p < 0.05).

Results

The outcomes showed lower UTS for CAP-P, control blend and MEP than MTEP, MDDP and MDP (p < 0.05). The degree of conversion was statistically similar for all resins (p = 0.122). On dentine, the wettability was higher (lower contact angle) with the most hydrophilic monomer MTEP. Higher WS was attained using MTEP. Different lengths of the spacer chains did not result in different wettability and WS (p > 0.05).

Conclusion

At similar molar percentage, different acidic functional monomers induced similar degree of conversion and different UTS when included in a 1-SEA. However, the inclusion of highly hydrophilic monomer may increase the wettability on dentine and the WS.     

Degree of conversion of three composite materials employed in the adhesive cementation of indirect restorations: A micro-Raman analysis

Objectives

Adhesive luting of indirect restorations can be carried out employing dual- or light-curing materials. This in vitro study evaluated the degree of conversion (DC) of the materials employed in this procedure, seeking how the combination of time and power of curing applied during polymerisation, as well as the temperature of the light-curing composite, influenced the DC.

Materials and methods

One hundred and eighty onlays of different thicknesses (2 mm, 3 mm, 4 mm) were luted with three different composites: two dual-curing cements (Variolink^® II and Calibra^®) and a light-curing composite (Venus^®). The same halogen lamp was used with three different modalities selected to provide a constant quantity of energy. The time/power combinations tested were 400 mW/cm² for 120 s, 800 mW/cm² for 60 s and 1200 mW/cm² for 40 s. The light-curing composite was employed at room temperature and after preheating at 54 °C. Each sample was examined in three positions using the Micro-Raman Dilor HR LabRam spectrometer to evaluate the polymer conversion degree. The data were analysed using analysis of variance and the Student–Newman–Keuls test (p = 0.05).

Results

The dual-curing materials showed average conversion percentages close to 64%, although onlays thickness clearly influence the degree of conversion, the light-curing composite showed satisfactory results only when onlays thickness was thin, however preheating significantly improved the performance of the light-curing composite under onlays of great thickness.

Conclusions

Optimal luting of indirect restorations is clearly dependent from light source power, irradiation time and dual-cure luting cement or light-curing composite chosen. It should be calibrated for each material to acquire high DCs. Preheating of light-curing only composites allows for the materials to reach optimal conversion degrees.     

Effect of temperature on composite polymerization stress and degree of conversion

Objective

To test the following hypotheses: (1) degree of conversion (DC) and polymerization stress (PS) increase with composite temperature (2) reduced light-exposure applied to pre-heated composites produces similar conversion as room temperature with decreased PS.

Methods

Composite specimens (diameter: 5 mm, height: 2 mm) were tested isothermally at 22 °C (control), 40 °C, and 60 °C using light-exposures of 5 or 20 s (control). DC was accessed 5 min after light initiation by FTIR at the specimen bottom surface. Maximum and final PS were determined, also isothermally, for 5 min on a universal testing machine. Non-isothermal stress was also measured with composite maintained at 22 °C or 60 °C, and irradiated for 20 s at 30 °C. Data were analyzed using two-way ANOVA/Tukey and Student's t-test (α = 5%).

Results

Both DC and isothermal maximum stress increased with temperature (p < 0.001) and exposure duration (p < 0.001). Isothermal maximum/final stress (MPa) were 3.4 ± 2.0b/3.4 ± 2.0A (22 °C), 3.7 ± 1.5b/3.6 ± 1.4A (40 °C) and 5.1 ± 2.0a/4.0 ± 1.6A (60 °C). Conversion values (%) were 39.2 ± 7.1c (22 °C), 50.0 ± 5.4b (40 °C) and 58.5 ± 5.7a (60 °C). The reduction of light exposure duration (from 20 s to 5 s) with pre-heated composite yielded the same or significantly higher conversion (%) than control (22 °C, 20 s/control: 45.4 ± 1.8b, 40 °C, 5 s s: 45.1 ± 0.5b, 60 °C, 5 s s: 53.7 ± 2.7a, p < 0.01). Non-Isothermal conditions showed significantly higher stress for 60 °C than 22 °C (in MPa, maximum: 4.7 ± 0.5 and 3.7 ± 0.4, final: 4.6 ± 0.6 and 3.6 ± 0.4, respectively).Clinical significance: Increasing composite temperature allows for reduced exposure duration and lower polymerization stress (both maximum and final) while maintaining or increasing degree of conversion.     

Heat curing of UTMA-based hybrid resin: effects on the degree of conversion and cytotoxicity

This study was designed to determine the effects of the heat curing time on a urethane tetramethacrylate (UTMA)-based hybrid resin and specifically on the degree of conversion (DC) and cytotoxicity. The materials used in this study were Estenia, a new-generation hybrid resin, and an experimental fiber reinforcement, Br-100. The DC values of the hybrid resin samples were measured using a Fourier transform infrared (FTIR) spectrophotometer after 180s of light curing followed by heat curing (0, 15, 30, and 60min). A method comparing intensities of C = C and N—H vibrations of the sample was used to calculate the final DC values. FTIR spectra were measured both inside and on the surface of the sample. The calculated DC values increased by increasing the heat curing times. After light curing only and after 15-min heat curing, the DC values inside the samples were smaller than the corresponding DC values at the surfaces of the samples. After 60min of heat curing, the samples achieved homogeneous polymerization (DC% = 65). The cytotoxicity of the material was studied from the glass fiber-reinforced hybrid resin samples, which were first light cured and then heat cured (15, 30, and 60min). Cytotoxicity was tested using both direct contact and extract methods. For the extract tests, the test specimens were incubated in a cell culture media at 37°, 54°, or 72°C for 24h. The heat curing times used had no effect on cytotoxicity. The incubation temperature, however, did have a significant effect. The extract obtained from 72°C incubation showed a cytotoxic effect whereas the others did not. The direct contact test did not show cytotoxicity.     

Prolonged exposure times of one-step self-etch adhesives on adhesive properties and durability of dentine bonds

Objectives

To evaluate the effect of prolonged exposure times on immediate and 6-month adhesive properties: degree of conversion (DC), nanoleakage (NL) and resin–dentine bond strength (μTBS) of three one-step self-etch adhesive systems (Adper Easy One [EO], Clearfil S³ Bond [CS3] and Go [GO]).

Material and methods

The adhesives were applied on exposed dentine surfaces of 90 human molars according to manufacturers’ instructions and light polymerized for 10, 20, and 40 s at 600 mW/cm². Bonded teeth were sectioned to obtain stick-shaped specimens (0.8 mm²) and tested under tensile stress (0.5 mm/min) immediately (IM) or after 6 months of water storage. Two bonded sticks from each tooth at each storage time interval were analysed by SEM for NL evaluation. The in situ DC was evaluated by micro-Raman spectroscopy. Data were analysed by appropriate ANOVA and Tukey's test (α = 0.05).

Results

Prolonged exposure times significantly increased the DC (%) (10 s [67.4 ± 17.3]; 20 s [85.9 ± 8.9] and 40 s [85.2 ± 9.0]) and decreased the NL (%) (10 s [24.8 ± 13.2]; 20 s [13.3 ± 7.5] and 40 s [13.5 ± 9.3]) for all adhesives; however it did not increase the IM μTBS for two (EO, GO) out of the three adhesives. Furthermore, this technique did not minimize dentine bond degradation.

Conclusion

Although longer exposure times than those recommended could not prevent degradation of dentine bonds, they could increase DC within the hybrid layer and reduced NL for all adhesives tested.