Effect of ceramic shade on the degree of conversion of a dual-cure resin cement analyzed by FTIR

Objectives: The aim of this research was to evaluate the degree of monomer conversion of different resin cement shades when photocured under different feldspathic ceramic shades. The photocuring time was also evaluated as well as the translucency of each ceramic shade. Methods: Three VITA VM7 ceramic shades (Base Dentin 0M1, Base Dentin 2M2 and Base Dentin 5M3) were used to determine the translucency percentage. A spectrophotometer MiniScan was used to measure the opacity percentage of each specimen (2-mm-thick) and then the translucency was calculated. To measure the degree of conversion (DC), the resin cement (Variolink II; A3 Yellow and transparent) specimens (thickness: 100 μm) were photocured under a ceramic block (2-mm-thick) for 20 or 40 s. Specimens photocured without the ceramic block were used as control. Sixteen groups (n = 3) were evaluated. Micro-ATR/FTIR spectrometry was used to evaluate the extent of polymerization of all specimens after 24 h. The %DC was calculated of experimentally polymerized versus maximally polymerized composite. Results: The translucency percentages of 0M1, 2M2 and 5M3 ceramics were 12.41 (1.02)%, 5.75 (1.91)% and 1.07 (0.03)%, respectively. The %DC of both resin cement shades cured under ceramic 5M3 was significantly lower than the other groups (p < 0.05). The %DC of 0M1 groups exhibited no significant difference from 2M2 groups (p > 0.05), with the exception of the transparent cement photocured for 40 s. Conclusion: Photocuring under 2 mm ceramic showed that the increase in chroma saturation significantly decreased Variolink II resin cement %DC (100-μm-thick). © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effects of cement-curing mode and light-curing unit on the bond durability of ceramic cemented to dentin

The aim of this study was to evaluate the effects of different light-curing units and resin cement curing types on the bond durability of a feldspathic ceramic bonded to dentin. The crowns of 40 human molars were sectioned, exposing the dentin. Forty ceramic blocks of VITA VM7 were produced according to the manufacturer's recommendations. The ceramic surface was etched with 10% hydrofluoric acid/60s and silanized. The dentin was treated with37% phosphoric acid/15s, and the adhesive was applied. The ceramic blocks were divided and cemented to dentin according to resin cement/RC curing type(dual-and photocured), light-curing unit (halogen light/QTH and LED), and storage conditions (dry and storage/150 days + 12,000 cycles/thermocycling). All blocks were stored in distilled water (37°C/24h) and sectioned (n = 10): G1-QTH + RC Photo, G2-QTH + RC Dual, G3-LED + RC Photo, G4-LED + RC Dual. Groups G5, G6, G7, and G8 were obtained exactly as G1 through G4, respectively, and then stored and thermocycled. Microtensile bond strength tests were performed (EMIC), and data were statistically analyzed by ANOVA and Tukey's test (5%). The bond strength values (MPa) were: G1-12.95 (6.40)ab; G2-12.02 (4.59)ab; G3-13.09 (5.62)ab; G4-15.96 (6.32)a; G5-6.22 (5.90)c; G6-9.48 (5.99)bc; G7-12.78 (11.30)ab; and G8-8.34 (5.98)bc. The same superscript letters indicate no significant differences. Different light-curing units affected the bond strength betweenceramic cemented to dentin when the photocured cement was used, and only after aging (LED>QTH). There was no difference between the effects of dual-and photo-cured resin-luting agents on the microtensile bond strength of the cement used in this study.

Durability of Adhesion between Feldspathic Ceramic and Resin Cements: Effect of Adhesive Resin, Polymerization Mode of Resin Cement, and Aging

Purpose: Adhesive cementation is an important step for restorations made of feldspathic ceramic as it increases the strength of such materials. Incorrect selection of the adhesive resin and the resin cement to adhere to the ceramic surface and their durability against aging can affect the adhesion between these materials and the clinical performance. This study evaluated the effect of adhesive resins with different pHs, resin cements with different polymerization modes, and aging on the bond strength to feldspathic ceramic. Materials and Methods: One surface of feldspathic ceramic blocks (VM7) (N = 90) (6.4 × 6.4 × 4.8 mm3) was conditioned with 10% hydrofluoric acid for 20 seconds, washed/dried, and silanized. Three adhesive resins (Scotchbond Multi-Purpose Plus [SBMP], pH: 5.6; Single Bond [SB], pH: 3.4; and Prime&Bond NT [NT], pH: 1.7) were applied on the ceramic surfaces (n = 30 per adhesive). For each adhesive group, three resin cements with different polymerization modes were applied (n = 10 per cement): photo-polymerized (Variolink II base), dual polymerized (Variolink II base + catalyst), and chemically polymerized (C&B). The bonded ceramic blocks were stored in water (37°C) for 24 hours and sectioned to produce beam specimens (cross-sectional bonded area: 1 ± 0.1 mm2). The beams of each block were randomly divided into two conditions: Dry, microtensile test immediately after cutting; TC, test was performed after thermocycling (12,000×, 5°C to 55°C) and water storage at 37°C for 150 days. Considering the three factors of the study (adhesive [3 levels], resin cement [3 levels], aging [2 levels]), 18 groups were studied. The microtensile bond strength data were analyzed using 3-way ANOVA and Tukey's post hoc test (α= 0.05). Results: Adhesive resin type (p < 0.001) and the resin cement affected the mean bond strength (p= 0.0003) (3-way ANOVA). The NT adhesive associated with the chemically polymerized resin cement in both dry (8.8 ± 6.8 MPa) and aged conditions (6.9 ± 5.9 MPa) presented statistically lower bond strength results, while the SBMP adhesive resin, regardless of the resin cement type, presented the highest results (15.4 to 18.5 and 14.3 to 18.9 MPa) in both dry and aged conditions, respectively (Tukey's test). Conclusion: Application of a low-pH adhesive resin onto a hydrofluoric acid etched and silanized feldspathic ceramic surface in combination with chemically polymerized resin cement did not deliver favorable results. The use of adhesive resin with high pH could be clinically advised for the photo-, dual-, and chemically polymerized resin cements tested. © 2012 by the American College of Prosthodontists.

Physicochemical and mechanical properties of zirconium oxide and niobium oxide modified Portland cement-based experimental endodontic sealers

Aim: To evaluate the physicochemical and mechanical properties of Portland cement-based experimental sealers (ES) with different radiopacifying agents (zirconium oxide and niobium oxide micro- and nanoparticles) in comparison with the following conventional sealers: AH Plus, MTA Fillapex and Sealapex. Methodology: The materials were tested for setting time, compressive strength, flow, film thickness, radiopacity, solubility, dimensional stability and formaldehyde release. Data were subjected to anova and Tukey tests (P < 0.05). Results: MTA Fillapex had the shortest setting time and lowest compressive strength values (P < 0.05) compared with the other materials. The ES had flow values similar to the conventional materials, but higher film thickness (P < 0.05) and lower radiopacity (P < 0.05). Similarly to AH Plus, the ES were associated with dimensional expansion (P > 0.05) and lower solubility when compared with MTA Fillapex and Sealapex (P < 0.05). None of the endodontic sealers evaluated released formaldehyde after mixing. Conclusion: With the exception of radiopacity, the Portland cement-based experimental endodontic sealers presented physicochemical properties according to the specifications no 57 ANSI/ADA (ADA Professional Product Review, 2008) and ISO 6876 (Dentistry - Root Canal Sealing Materials, 2012, British Standards Institution, London, UK). The sealers had setting times and flow ability that was adequate for clinical use, satisfactory compressive strength and low solubility. Additional studies should be carried out with the purpose of decreasing the film thickness and to determine the ideal ratio of radiopacifying agents in Portland cement-based root canal sealers. © 2013 International Endodontic Journal.

Calcium aluminate cement: Used in bone defects induced in the femur of rabbits

The patterns of the calcium aluminate cement in bone defects experimentally induced in the femur of 12 New Zealand White rabbits were evaluated. The animals were distributed in three experimental groups, corresponding to postoperative observation periods of 15 (G15), 30 (G30) and 60 (G60) days. Clinical, surgical, radiographic and histological appraisals were made to observe the osteoinductor and osteoconductor potential of the biological material, as well as the bone integration. The calcium aluminate cement formulation was biocompatible, but has not acted as a osteoconductor or osteoinductor.

Degree of conversion and hardness of two different systems of the vitrebond™ glass ionomer cement light cured with blue LED

This study investigated the physicochemical properties of the new formulation of the glass ionomer cements through hardness test and degree of conversion by infrared spectroscopy (FTIR). Forty specimens (n = 40) were made in a metallic mold (4 mm diameter × 2 mm thickness) with two resin-modified glass ionomer cements, Vitrebond™ and Vitrebond™ Plus (3M/ ESPE). Each specimen was light cured with blue LED with power density of 500 mW/cm2during 30 s. Immediately after light curing, 24h, 48h and 7 days the hardness and degree of conversion was determined. The Vickers hardness was performed by the MMT-3 microhardness tester using load of 50 gm force for 30 seconds. For degree of conversion, the specimens were pulverized, pressed with KBr and analyzed with FT-IR (Nexus 470). The statistical analysis of the data by ANOVA showed that the Vitrebond™ and Vitrebond™ Plus were no difference significant between the same storage times (p > 0.05). For degree of conversion, the Vitrebond™ and Vitrebond™ Plus were statistically different in all storage times after light curing. The Vitrebond™ showed higher values than Vitrebond™ Plus (p < 0.05). The performance of Vitrebond™ had greater results for degree of conversion than Vitrebond™ Plus. The correlation between hardness and degree of conversion was no evidence in this study.

Si-based thin film coating on Y-TZP: Influence of deposition parameters on adhesion of resin cement

This study evaluated the influence of deposition parameters for Si-based thin films using magnetron sputtering for coating zirconia and subsequent adhesion of resin cement. Zirconia ceramic blocks were randomly divided into 8 groups and specimens were either ground finished and polished or conditioned using air-abrasion with alumina particles coated with silica. In the remaining groups, the polished specimens were coated with Si-based film coating with argon/oxygen magnetron discharge at 8:1 or 20:1 flux. In one group, Si-based film coating was performed on air-abraded surfaces. After application of bonding agent, resin cement was bonded. Profilometry, goniometry, Energy Dispersive X-ray Spectroscopy and Rutherford Backscattering Spectroscopy analysis were performed on the conditioned zirconia surfaces. Adhesion of resin cement to zirconia was tested using shear bond test and debonded surfaces were examined using Scanning Electron Microscopy. Si-based film coating applied on air-abraded rough zirconia surfaces increased the adhesion of the resin cement (22.78 ± 5.2 MPa) compared to those of other methods (0-14.62 MPa) (p = 0.05). Mixed type of failures were more frequent in Si film coated groups on either polished or air-abraded groups. Si-based thin films increased wettability compared to the control group but did not change the roughness, considering the parameters evaluated. Deposition parameters of Si-based thin film and after application of air-abrasion influenced the initial adhesion of resin cement to zirconia. © 2013 Elsevier B.V. All rights reserved.

Retenção do cátion do sulfato de cobre nos compartimentos biótico e abiótico de mesocosmos com sistema de fluxo contínuo de água

Pós-graduação em Aquicultura - FCAV

Preparation of refractory calcium aluminate cement using the sonochemical process

Calcium aluminate cements (CAC) were prepared using the sonochemical process, followed by heat treatment. A study was made of the action of ultrasonic waves and the influence of thermal treatment conditions on two initial molar compositions of 1:1 and 1:2 of calcia:alumina. The aqueous suspension containing the raw materials (A-50 alumina and CaO) was subjected to an ultrasonic bath, followed by drying and burning at 1000, 1200 and 1300 ºC. These cements were characterized by SEM, XRD and the mechanical strength was evaluated by splitting tensile tests, using commercial cement as a reference. Furthermore, the phases were semi-quantified using the Rietveld method. The results show that hydration and sonochemical action increased the reactivity of the raw materials during firing and that phase formation is dependent on the thermal treatment conditions. The CAC cements were obtained at temperatures at least 200 ºC lower than those used in conventional methods, indicating the potential of this route of synthesis.

Comparison of Physicochemical Surface Conditioning Methods for Adhesion of bis-GMA Resin Cement to Particulate Filler Composite and Surface Characterization

This study compared the effect of physicochemical surface conditioning methods on the adhesion of bis-GMA-based resin cement to particulate filler composite (PFC) used for indirect dental restorations. PFC blocks (N (block)=54, n (block)=9 per group) were polymerized and randomly subjected to one of the following surface conditioning methods: a) No conditioning (Control-C), b) Hydrofluoric acid (HF)etching for 60s (AE60), c) HF for 90s (AE90), d) HF for 120s (AE120), e) HF for 180s (AE180), and f) air-abrasion with 30 mu m silica-coated alumina particles (AB). The conditioned surfaces were silanized with an MPS silane, and an adhesive resin was applied. Resin composite blocks were bonded to PFC using resin cement and photo-polymerized. PFC-cement-resin composite blocks were cut under coolant water to obtain bar specimens (1mmx0.8mm). Microtensile bond strength test (mu TBS)was performed in a universal testing machine (1mm/min). After debonding, failure modes were classified using stereomicroscopy. Surface characterization was performed on a set of separate specimen surfaces using Scanning Electron Microscopy (SEM), X-Ray Dispersive Spectroscopy (XDS), X-Ray Photoelectron Spectroscopy (XPS), and Fourier Transform-Raman Spectroscopy (FT-RS). Mean mu TBS (MPa) of C (35.6 +/- 4.9) was significantly lower than those of other groups (40.2 +/- 5.6-47.4 +/- 6.1) (p<0.05). The highest mu TBS was obtained in Group AB (47.4 +/- 6.1). Prolonged duration of HF etching increased the results (AE180: 41.9 +/- 7), but was not significantly different than that of AB (p>0.05). Failure types were predominantly cohesive in PFC (34 out of 54) followed by cohesive failure in the cement (16 out of 54). Degree of conversion (DC) of the PFC was 63 +/- 10%. SEM analysis showed increased irregularities on PFC surfaces with the increased etching time. Chemical surface analyses with XPS and FT-RS indicated 11-70% silane on the PFC surfaces that contributed to improved bond strength compared to Group C that presented 5% silane, which seemed to be a threshold. Group AB displayed 83% SiO2 and 17% silane on the surfaces.

Stress distribution on dentin-cement-post interface varying root canal and glass fiber post diameters. A three-dimensional finite element analysis based on micro-C data

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Bond Strength of Different Resin Cement and Ceramic Shades Bonded to Dentin

Purpose: To evaluate the microtensile bond strength (MTBS) of ceramic cemented to dentin varying the resin cement and ceramic shades.Materials and Methods: Two VITA VM7 ceramic shades (Base Dentine 0M1 and Base Dentine 5M3) were used. A spectrophotometer was used to determine the percentage translucency of ceramic (thickness: 2.5 mm). For the MTBS test, 80 molar dentin surfaces were etched and an adhesive was applied. Forty blocks (7.2 x 7.2 x 2.5 mm) of each ceramic shade were produced and the ceramic surface was etched (10% hydrofluoric acid) for 60 s, followed by the application of silane and resin cement (A3 yellow and transparent). The blocks were cemented to dentin using either A3 or transparent cement. Specimens were photoactivated for 20 s or 40 s, stored in distilled water (37 degrees C/24 h), and sectioned. Eight experimental groups were obtained (n = 10). Specimens were tested for MTSB using a universal testing machine. Data were statistically analyzed using ANOVA and Tukey's post-hoc tests (alpha <= 0.05).Results: The percentage translucency of 0M1 and 5M3 ceramics were 10.06 (+/- 0.25)% and 1.34 (+/- 0.02)%, respectively. The lowest MTBS was observed for the ceramic shade 5M3. For the 0M1 ceramic, the A3 yellow cement that was photocured for 20 s exhibited the lowest MTBS, while the transparent cement that was photocured for 40 s presented the highest MTBS.Conclusions: For the 2.5-mm-thick 5M3 ceramic restorations, the MTBS of ceramic cemented to dentin significantly increased. The dual-curing cement Variolink II photocured for 40 s is not recommended for cementing the Base Dentine 5M3 feldspathic ceramic to dentin.

Can Heat Treatment Procedures of Pre-hydrolyzed Silane Replace Hydrofluoric Acid in the Adhesion of Resin Cement to Feldspathic Ceramic?

Purpose: To evaluate the influence of heat treatment (HT) procedures of a pre-hydrolyzed silane on bond strength of resin cement to a feldspathic ceramic.Materials and Methods: Ceramic and composite blocks (N = 30) were divided into six groups (n = 5) and subjected to the following conditioning procedures: G1: 9.6% hydrofluoric acid (HF) for 20 s + silane (RelyX Ceramic Primer, 3M ESPE) + resin cement (Panavia F2.0, Kuraray) (control); G2: HF (20 s) + silane + heat treatment in furnace (HTF) (100 degrees C, 2 min) + resin cement; G3: silane + HTF + resin cement; G4-HF (20 s) + silane + heat treatment with hot air (HTA) (50 +/- 5 degrees C for 1 min) + resin cement; G5: silane + HTA + resin cement; G6: silane + resin cement. The microtensile bond strength (MTBS) test was performed using a universal testing machine (1 mm/min). After debonding, the substrate and adherent surfaces were analyzed using a stereomicroscope and SEM to categorize the failure types. The data were statistically evaluated using one-way ANOVA and Tukey's test (5%).Results: The control group (G1) showed no pre-test failures and presented significantly higher mean MTBS (16.01 +/- 1.12 MPa) than did other groups (2.63 +/- 1.05 to 12.55 +/- 1.52 MPa) (p = 0.0001). In the groups where HF was not used, HTF (G3: 12.55 +/- 1.52 MPa) showed significantly higher MTBS than did HTA (G5: 2.63 +/- 1.05 MPa) (p < 0.05). All failure types were mixed, ie, adhesive between the resin cement and ceramic accompanied by cohesive failure in the cement.Conclusion: Heat treatment procedures for the pre-hydrolyzed silane either in a furnace or with the application of hot air cannot replace the use of HF gel for the adhesion of resin cement to feldspathic ceramic. Yet when mean bond strengths and incidence of pre-test failures are considered, furnace heat treatment delivered the second best results after the control group, being considerably better than hot air application.

Effect of Post-silanization Heat Treatments of Silanized Feldspathic Ceramic on Adhesion to Resin Cement

Purpose: To evaluate the effect of post-silanization heat treatment of a silane agent and rinsing with hot water of silanized CAD/CAM feldspathic ceramic surfaces on the microtensile bond strength between resin cement and the ceramic, before and after mechanical cycling.Materials and Methods: Blocks measuring 10 x 5.7 x 3.25 mm(3) were produced from feldspathic ceramic cubes (VITA Mark II, VITA Zanhfabrik). Each ceramic block was duplicated in composite resin using a template made of polyvinylsiloxane impression material. Afterwards, ceramic and corresponding resin composite blocks were ultrasonically cleaned and randomly divided according to the 5 strategies used for conditioning the ceramic surface (n = 10): GHF: etching with hydrofluoric acid 10% + rinsing with water at room temperature + silanization at 20 degrees C; G20: silanization; G77: silanization + oven drying at 77 degrees C; G20r: silanization + hot water rinsing; G77r: silanization + oven drying at 77 C + hot water rinsing. The resin and ceramic blocks were cemented using a dual-curing resin cement. Every group was divided in two subgroups: aging condition (mechanical cycling, designated as a) or non-aging (designated as n). All the bonded assemblies were sectioned into microsticks for microtensile bond strength (mu TBS) testing. The failure mode of the tested specimens was assessed and mu TBS data were statistically analyzed in two ways: first 2-way ANOVA (GHF, G20 and G77 in non-aging/aging conditions) and 3-way ANOVA (temperature x rinsing x aging factors, excluding GHF), followed by Tukey's test (p = 0.05).Results: The 2-way ANOVA revealed that the mu TBS was significantly affected by the surface treatment (p < 0.001) but not by aging (p = 0.68), and Tukey's test showed that G77-n/G77-a (18.0 MPa) > GHF-n/GHF-a (12.2 MPa) > G20-n/G20-a (9.1 MPa). The 3-way ANOVA revealed that the mu TBS was significantly affected by the heat treatment and rinsing factors (p < 0.001), but not affected by aging (p = 0.36). The rinsing procedure decreased, while oven drying increased the bond strengths. Group G77, in both non-aging and aging conditions (18.6-17.4 MPa), had the highest bond values. Failure modes were mainly mixed for all groups.Conclusion: Oven drying at 77 degrees C improved the bond strength between the resin cement and feldspathic ceramic, but hot water rinsing reduced the bond strength and should not be recommended.