Interfacial shear strength of C/C composites

Fiber-bundle push-out, single-fiber push-in, and single-fiber push-out tests were conducted in order to examine the applicability of these methods for determining the interfacial shear strength of carbon-carbon composites. The fiber-bundle push-out test resulted mostly in fractures along the fiber/matrix interface but created a small amount of fractures in the matrix. Hence, the evaluated strength was regarded as an approximate value. In order to precisely evaluate the interfacial strength, push-in and push-out tests for a single fiber were performed using a micro-Vickers indentation tester. In these tests, the load has to be placed within a target fiber, and the indentation should not extend to the matrix. This condition restricted the load that could be applied to a carbon fiber. Within this limit, a single carbon fiber could not be pushed-in. For the sake of load reduction, single-fiber push-out tests were conducted using thin specimens. The thickness appropriate for a single-fiber push-out specimen was estimated based on the interfacial shear strength obtained by the bundle push-out tests. Below this thickness, single-fiber push-out tests could be successfully performed.     

Effect of the interfacial area measurement parameters on the push-out strength between fiber post and dentin

PurposeTo verify the influence of different instruments and operators on the bonding interfacial area and on the push-out bond strength values.Material and methodsFifteen anterior human teeth (n=15) were selected, cleaned and standardized to 15 mm length. Root canals were prepared in 12 mm and the fiber posts were cemented using the RelyX U-100 cement. Three slices were obtained per tooth (N=45) and submitted to the push-out bond strength test. The bonding interfacial area (mm²) of each specimen was calculated based on the disc slice dimensions: coronal and apical diameter and height. The bonding area of each specimen was used to calculate the bond strength (Mpa). The dimensions were analyzed by different operators, using two instruments: G1 – Operator A with a digital caliper; G2 – Operator A with a stereomicroscope; G3 – Operator B with a digital caliper; G4 – Operator B with a digital stereomicroscope; G5 – Operator C with a digital caliper; G6 – Operator C with a stereomicroscope. The mean area was submitted to inter-operator and intra-operator analyses, while the mean area and mean of bond strength were submitted to the 2-way ANOVA with repeated measures and the Tukey test (α=0.05).ResultsThe inter-operator kappa was 0.83 to the digital caliper and 0.91 to the stereomicroscope, while the intra-operator kappa was 0.76. The operator and the measurement instrument influenced the interfacial bonding area (p=0.000 and p=0.001) and the push-out bond strength values (p=0.000 and p=0.000, respectively) of the disc slices.ConclusionThe final push-out bond strength values are influenced by the measuring instrument and by the measurer operator.     

Influence of the ER,CR:YSGG laser and different irrigation methods on push-out bond strength of fiber post

Er,Cr:YSGG lasers are currently being investigated for disinfecting the root canal treatment. The aim of this study was to compare the effects of various irrigation protocols on push-out bond strength of fiber posts. Fifty maxillary anterior teeth were divided into five groups (n = 10) according to the protocol that applied into the post space. Group-1: distilled water, Group-2: 5% NaOCl, Group-3: 2% CHX, Group-4: Er,Cr:YSGG laser (1.5 W, 20 Hz, 85 air, 75 water, 26.7 J/cm²), Group-5: Er,Cr:YSGG laser (1.25 W, 50 Hz, 34 air, 24 water, 12.7 J/cm²). Fiber posts were cemented with resin cement. The remaining part of the root, three slices were obtained from each specimen and push-out test was performed. One-way ANOVA and Duncan’s test at a 5% level of significance were used for the statistical analysis. Post space irradiation with Er,Cr:YSGG laser (1.5 W 20 Hz, 85 air, 75 water, 26.7 J/cm²) increases push-out bond strength of fiber post to root canal dentin. Further investigations are needed to establish and optimize ER,Cr:YSGG laser parameters to increase the push-out bond strength of fiber posts.     

Mechanical properties of flared root canals restored with fiber post and chemically activated resin: study using push-out bond strength and fracture load tests

This study aimed to evaluate the fracture load and push-out bond strength of flared root canals restored with different procedures, including a technique with a fiber post and a chemically activated resin composite. Eighty human canines were selected and treated endodontically. Two methodologies were used: push-out and fracture load. The teeth were divided into four groups: Cast metal core (CMC); PAN (direct anatomic post); PAC (fiber post and accessory posts); and PE (fiber post with chemically activated resin composite). For the fracture load test, the samples were submitted to load application in a universal testing machine. The fracture mode was evaluated visually. Forty other samples were submitted to the push-out test. The fracture load (n = 10) and the bond strength (n = 10) were analyzed by analysis of variance and Tukey tests (α < 0.05). CMC presented the highest fracture load (p < 0.05), and no significant differences were observed in the fracture load values for Groups PAN, PAC, and PE. CMC presented 90% of unfavorable failures; PAN and PAC, the remaining 10% of these failures. PE presented only favorable failures. PAC presented lower push-out bond strength values. The fracture load for CMC procedure was higher than that of the others, but presented 90% unfavorable fractures, indicating the use of any of the glass fiber post techniques evaluated for restoring flared root canals due to favorable fracture modes.     

Effect of the frequency of mechanical pulses for fatigue aging testing on push-out bond strength between glass fiber posts and root dentin

The aim of this study was to evaluate the influence of the frequency of mechanical pulses during mechanical fatigue aging on bond strength between glass fiber posts and root dentin. Fiber posts were adhesively cemented in 30 bovine roots and the core was built up with composite. All specimens were subjected to mechanical cycling (45° angle; 37 °C; 50 N; 2×10⁶ pulses) at different frequencies: 2, 4, and 8 Hz. After the fatigue, each specimen was submitted to push out test. The bond strength was calculated for data analysis (one-way ANOVA, p = 0.05). The frequency did not affect the push-out (p = 0.7). The main failure mode was between dentin and cement in all groups. The mechanical pulses were not influenced by the bond strength between root dentin and fiber posts. Thus, it is possible to decrease the time-consuming in vitro tests involving posts without damaging the reliability of the test.     

The Disk-Specimen Thickness Does Not Influence the Push-Out Bond Strength Results Between Fiber Post and Root Dentin

This study evaluated the effect of different thickness of disk-shaped specimens on the push-out bond strength test. Eighteen lower bovine teeth were sectioned (20 mm) and prepared (15 mm) with the same post system drill (Light Post® #1, Schaumburg, IL, Bisco, USA). The apical third of each specimen was embedded in a plastic matrix filled with an acrylic resin (Dencrilay?, Dencril, Sao Paulo, Brazil). The posts were cleaned with alcohol, silanated (ProSil®, FGM, Joenville, SC, Brazil) and cemented with the RelyX? U100 (3 M ESPE, St. Paul, MN, USA). Each specimen was sectioned into three pieces of differing thicknesses (1, 2, and 4 mm). These disk-samples were allocated into 3 groups (n = 18) and subjected to push-out testing. One-way ANOVA showed no influence of the specimen thickness on the results (p = 0.842). No correlation was observed between thickness and push-out bond strength (Pearson Correlation, r² = 0.0688; P = 0.6209). The push-out bond strength test was not affected by the thickness of the disk-specimens.     

Influence of storage time on bond strength of self-etching adhesive systems to artificially demineralized dentin after a papain gel chemical–mechanical agent application

ObjectivesThe aim of this study was to evaluate the influence of storage time on the bond strength of self-etching adhesive systems to artificially demineralized dentin submitted to application of a papain-based chemical mechanical agent for carious tissue removal.Materials and MethodsTwenty-four blocks of human coronal dentin were randomly divided into 2 groups: (1) restored with a two-step self-etching adhesive system (Clearfil SE Bond); (2) restored with a one-step self-etching adhesive system (One-Up Bond F Plus). After artificial caries induction, the specimens were treated with papain-based gel, received an application of the adhesive system according to the respective group, and blocks of microhybrid resin composite measuring 5.0 mm high and 5.0 mm wide were fabricated incrementally on the tooth, which would later be cut to obtain sticks with a bond area of around 1 mm², for use in the microtensile tests. After this, half of the sticks obtained from each tooth were submitted to the microtensile test 24 h later, while the other half were stored in water, in an oven at 37° C for a period of 180 d. The specimens were submitted to the microtensile test in a Universal Test Machine at a speed of 0.5 mm/min. The surfaces of the fractured test specimens were examined visually under a stereoscopic loupe in order to classify the fracture type. After exploratory analysis of the data, the two-way Analysis of Variance (ANOVA) and the Tukey test were applied. The data on the fracture types were analyzed by the Exact Fisher test.ResultsNo statistically relevant differences were verified among the means of the microtensile bond strength values of the adhesive systems evaluated in the different storage times. Mixed and adhesive fractures types were observed for both groups.ConclusionStorage time did not influence the bond strength of the two-step or one-step self-etching adhesive systems to artificially demineralized dentin submitted to application of a papain-based chemical mechanical agent for carious tissue removal. Both adhesive systems provided similar bond strength at different storage times.     

The effect of post surface silanization and luting agents on the push-out bond strengths of adhesively inserted fiber reinforced posts

The effect of silane treatment on the push-out bond strengths of three different luting agents to fiber-reinforced composite (FRC) posts after thermocycling was evaluated.Sixty single-rooted human maxillary central incisors were sectioned below the cemento-enamel junction, and the roots were endodontically treated. RelyX Fiber Posts (size #2) were inserted using etch-and-rinse, self-etch, and self-adhesive luting agents (cementing agents). For half of the specimen in each group, the fiber posts were treated with a silane coupling agent. Bonded specimens were cut (2-mm-thick sections) and push-out tests were performed (crosshead speed, 0.5 mm/min). Failure modes were evaluated using a stereomicroscope at original magnification ×40.For each luting agent the use of silane did not result in any statistically significant difference at any level of the root compared to those of the control groups except for Variolink II and RelyX Unicem luting agents in apical root section (p<0.05; one-way ANOVA). The post hoc analysis showed that regardless of the pre-treatment procedures, Variolink II achieved significantly higher bond strengths than Panavia F 2.0 and RelyX Unicem in all root sections (p<0.05).The use of a silane coupling agent had no influence on bond strengths depending on the luting agent used, whereas the type of luting agent (etch-and-rinse, self-etch, and self-adhesive) appeared to be a significant influence on the push-out bond strength values independent of the pre-treatment used. Therefore, pre-treatment of fiber posts with a silane coupling agent does not seem to be mandatory, which saves time in the clinical situation.     

The effects of chelation on the adhesion of two different root canal sealers

Objective: This study aims to evaluate alterations in the root canal dentin after irrigation with EDTA, HEBP, and Chitosan in order to determine the push-out bond strengths of the different root canal sealers on altered dentin surfaces. Materials And Methods: Crowns of 70 maxillary single-rooted teeth were removed to obtain a standardized length of 16 mm. The canals were instrumented using rotary files and the step back technique. The master apical file used in this study was #40. The subgroups were determined based on the chelation agent and the material of the root canal sealer that was used (17% EDTA, 18% HEPB, 0.2% Chitosan, Well Root ST (WRST) or AH Plus). Three slices with 1 mm thickness were cut from the root thirds of each tooth and subjected to a push-out test. The data (MPa) were analyzed using a one-way ANOVA and a Duncan’s multiple comparison test at a level of α = 0.05. Finally, scanning electron microscope (SEM) photographs were taken. Results: Groups that used WRST exhibited significantly higher push-out bond strength values in all subgroups independent of the irrigant that was used (ANOVA, p < 0.05). Group 1 showed higher push-out bond strength than the other AH Plus subgroups. Conclusion: The EDTA improved the push-out bond strength of the AH Plus. The WRST root canal sealer had the highest push-out bond strength and did not depend on the irrigant used.     

Experimental techniques for measuring fibre/matrix interfacial bond shear strength

Experimental techniques for directly obtaining some measure of the shear strength of the interfacial bond between fibrous reinforcements and cemetitious matrices are reviewed. These techniques— essentially single- or multiple-fibre pull-out out tests — are classified according to specimen type and configuration and are then evaluated and compared using a set of criteria adapted by the author for this purpose. None of the techniques are found to satisfy completely all of the criteria, but several probably could be modified to do so. The objective of this state-of-the-art review is to provide a basis for discussion of the possible future standardization of a test technique for determining fibre/matrix interfacial bond shear strength in cementitious matrix composite specimens.     

Effect of Er,Cr:YSGG laser surface conditioning on the adhesion of fiber- reinforced composite and zirconia intraradicular posts to the root dentin

This study evaluated the influence of Er,Cr:YSGG laser surface conditioning on push-out bond strength of different root posts to the root dentin. Extracted (N = 27, n = 9 per group) and endodontically treated human mandibular premolars were prepared to receive the posts. Three types of posts, namely quartz fiber (D), glass fiber (S), and zirconium dioxide post (C) were luted with resin cement. The posts were randomly assigned to one of the surface conditioning method: (a) No conditioning, control (L0), (b) Er,Cr:YSGG laser at 175 mJ, 3.5 W for 60 s (L1), and (c) at 225 mJ, 4.5 W for 60 s, with 60 μs pulse duration and repetition rate was 20 Hz (L2) irradiation. Six sections (two coronal, two middle, and two apical) were made in each tooth yielding to 1 mm thick specimens. The specimens were stored in distilled water at 37?°C for 24 h and push-out bond strength (MPa) was tested in a Universal Testing Machine (1 mm/min). Data were analyzed using Kruskall–Wallis and Dunns`s post hoc tests (α = 0.05). In group D, both laser treated groups (L1:16.16 ± 19.89; L2:8.24 ± 9.26) presented significantly less bond strength compared to control group (L0:28.3 ± 16.8) (p < 0.001). Mean push-out bond strength values did not significantly differ according to the root segments (coronal, middle, and apical) (p = 0.106). Application of Er,Cr:YSGG laser, with the parameters tested, did not increase the bond strength of zirconium glass fiber and zirconium oxide posts. Laser surface conditioning decreased the bond strength of quartz fiber posts in the root canal.     

Bond strength measurement between glass fibres and epoxy resin at elevated temperatures using the pull-out and push-out techniques

Pull-out and push-out measurements were performed on glass fibres in an epoxy resin to determine the dependence of bond strength on test temperature and on fibre surface treatment. A comparative analysis of the two techniques was carried out to elucidate elementary processes of polymer-fibre debonding and to determine energy values for adhesional bonds. Differences in bond strength values for pull-out and push-out tests were attributed to failure mechanisms that were either interface-controlled or matrix-controlled. Evidence for the different failure mechanisms characteristic of the two test techniques was provided by an estimation of failure parameters, such as the activation energy for debonding. Failure mechanisms also were manifest in AFM images, showing differences in topography and roughness that depended on fibre surface treatment, test geometry, and test temperature.     

BOND STRENGTH MEASUREMENT BETWEEN GLASS FIBRES AND EPOXY RESIN AT ELEVATED TEMPERATURES USING THE PULL-OUT AND PUSH-OUT TECHNIQUES

Pull-out and push-out measurements were performed on glass fibres in an epoxy resin to determine the dependence of bond strength on test temperature and on fibre surface treatment. A comparative analysis of the two techniques was carried out to elucidate elementary processes of polymer-fibre debonding and to determine energy values for adhesional bonds. Differences in bond strength values for pull-out and push-out tests were attributed to failure mechanisms that were either interface-controlled or matrix-controlled. Evidence for the different failure mechanisms characteristic of the two test techniques was provided by an estimation of failure parameters, such as the activation energy for debonding. Failure mechanisms also were manifest in AFM images, showing differences in topography and roughness that depended on fibre surface treatment, test geometry, and test temperature.     

Tensile Properties of Arenga pinnata Fiber-Reinforced Epoxy Composites

The aim of this study is to determine the tensile properties of Arenga pinnata fiber as a natural fiber and epoxy resin as a matrix. The Arenga pinnata fibers were mixed with epoxy resin at the various fiber weight percentages of 10%, 15%, and 20% Arenga pinnata fiber and with different fiber orientations such as long random, chopped random, and woven roving. Hand lay-up processes in this experiments were to produce specimen test with the curing time for the composite plates is in the room temperature (25–30°C). Results from the tensile tests of Arenga pinnata fiber reinforced epoxy composite are that the 10 wt.% woven roving Arenga pinnata fiber showed the highest value for maximum tensile properties. The tensile strength and Young's modulus values for 10 wt.% of woven roving Arenga pinnata fiber composite are 51.725 MPa and 1255.825 MPa, respectively. The results above indicate that the woven roving Arenga pinnata fiber has a better bonding between its fiber and matrix compared to long random Arenga pinnata fiber and chopped random Arenga pinnata fiber. Scanning electron microscopy (SEM) tests were carried out after tensile tests to observe the interface of fiber and matrix adhesion.     

纤维与水泥砂浆界面黏结性能研究

本文采取“8字”型试件进行单根粗纤维拉拔试验,通过混合正交试验研究了纤维类型、纤维直径、纤维埋置长度及砂浆基体水胶比对纤维-砂浆界面黏结强度显著性优先次序,以及纤维与砂浆间最佳组合的影响。同时得到了纤维最大拔出荷载及荷载-滑移曲线,系统分析了纤维与水泥砂浆的界面黏结性能。试验结果表明,直径为0.6 mm、埋置长度为20 mm的聚丙烯粗纤维,水胶比为0.51的砂浆基体的界面黏结强度最大,其中平均黏结强度为7.71 MPa,等效黏结强度达到13.25 MPa。直径为0.6 mm、埋置长度为10 mm的聚乙烯醇(PVA)纤维,水胶比为0.41的砂浆基体的界面黏结强度次之。四种因素对界面黏结强度的影响优先次序为纤维种类、纤维直径、砂浆水胶比、纤维埋置长度,其中纤维种类对界面平均黏结强度的影响较为显著,纤维直径对界面等效黏结强度的影响较为显著。     

Impact of conditioning regimens and time on adhesion of a fiber post to root dentin using two resin cements

The aim of this study was to evaluate the influence of irrigation protocols on the bond strength of a glass fiber post bonded to dentin using two resin cements. In 200 root-filled teeth, post space was prepared and divided into five groups (n?=?40) based on the irrigation protocol: group 1 (3% sodium hypochlorite), group 2 (3% sodium hypochlorite – 17% Ethylene diamine tetraacetic acid), group 3 (a mixture of sodium hypochlorite and etidronic acid), group 4 (sodium hypochlorite – QMix), and group 5 (distilled water). Samples were subdivided into two subgroups (n?= 10) and fiber posts were cemented using subgroup A (Self-adhesive dual-cure resin cement; SEA) or B (dual-cure resin cement following an etch-and-rinse protocol, ER). Push-out bond strength was performed after 24 h and four months (n?= 10) and failure modes were categorized. Statistical analysis of data was carried out by appropriate analyses (p < 0.05). The irrigation protocol and the resin cement had a significant impact on push-out bond strength. Subgroup A group showed lower bond strength than B at both time periods when 3% NaOCl–17% EDTA and 1:1 mixture of 6% NaOCl + 18%EA protocols were used. Three percent NaOCl used in combination with 17% EDTA or QMix significantly decreased the push-out bond strength of ER at the end of four months (p < 0.05). In conclusion, dual-cure resin cements bonded with etch-and-rinse protocol showed highest bond strength when a mixture of NaOCl and etidronic acid was used as root canal irrigant. These values were differentially influenced by time.     

Evaluation of the Microtensile Bond Strength between Resin Composite and Hydrofluoric Acid Etched Ceramic in Different Storage Media

The aim of this study was to evaluate the effects of storage media on the bond strength between resin composite and ceramic that was etched with hydrofluoric acid and silanized. Two types of ceramics were used: lithium disilicate and leucite-reinforced. The ceramic surface was etched with 4.7% hydrofluoric acid and bonded to the resin composite using a silane coupling agent. Specimens were divided into 10 groups and each group of specimen was subjected to different types of storage conditions for 7 days: de-ionized water (control), 15% ethanol, lemon soda, and cola. The microtensile test was used to measure the bond strength. The results showed that storage in food beverages significantly reduced bond strength compared to controls because of the acidity of beverages (ANOVA; p < 0.05). Lithium disilicate ceramics stored for 7 days in ethanol produced bond strengths significantly lower than those stored in 7 days in de-ionized water (p < 0.05). Leucite-reinforced ceramics stored for 7 days in lemon soda generated mean bond strengths significantly lower than those stored for 7 days in de-ionized water (p < 0.05). The significance of this in vitro study is that patients who have just repaired fractured crowns or inserted laminates should refrain from drinking acidic substances because it may weaken the resin-to-ceramic bond.     

Shrinkage stress,long-term adaptation and bond strength of low-shrinkage composite resins

PurposeTo evaluate the internal adaptation, bond strength, and polymerization stress of silorane- and methacrylate-based composite resins.Material and methodsThree methacrylate-based composite resins (Heliomolar; Tetric N-Ceram and Aelite LS) and one silorane-based composite resin (Filtek Silorane) were tested. Polymerization stress (n=5) was determined by the insertion of the composite resin between rods of polymethyl methacrylate. The ratio of the maximum force of contraction was recorded and the cross-sectional area of the rod was used to calculate the nominal stress. Bond strength was evaluated by microtensile bond test. Dentin surfaces of human third molars were bonded, sectioned, and stored for 24 h or 1 year in distilled water before the bond strength test. The ratio of maximum force and the adhered area was used for the bond strength calculation. For internal adaptation analysis, third molars received Class II cavities and were restored according to either an incremental oblique or bulk-filling technique. After being sectioned perpendicularly, impressions were taken and epoxy resin replicas were obtained of the internal surfaces of the restorations (after 24 h and 1 year of storage) to analyze gap formation using scanning electron microscopy.ResultsFiltek Silorane showed the highest​ bond strength after one year of storage, the lowest formation of gaps, and polymerization stress similar to methacrylate-based materials.ConclusionSilorane restorative material presented polymerization stress comparable to that of methacrylate-based composite resins, stable dentin bond strength after one year and better internal adaptation to the cavity walls, showing good alternative to traditional composite resins and promising longevity.     

Endodontic irrigants effect on long-term intraradicular adhesion of resin cements

The aim of this study was to evaluate over time the bond strength of dual-cure and self-adhesive resin cements used for bonding fiberglass posts following irrigation with different solutions. Ninety roots from single-rooted premolars were selected and divided into 6 groups (n = 15) according to the resin cement, dual-cure or self-adhesive (RelyX ARC and RelyX U100) or the endodontic irrigant used (2% chlorhexidine digluconate - CH, 1% sodium hypochlorite - SH and deionized distilled water – control). Following post cementation, the roots were cross-sectioned in order to obtain two slices from each root third (cervical, mid and apical). The specimens were stored for 7 or 180 days in water and the push-out bond strength test applied. The data was analyzed using three-way ANOVA and Tukey Kramer. The interaction endodontic irrigants-resin cement vs. storage time was significant (p = 0.008), where 7 days of storage induced no difference between the groups, however, after 180 days, the groups for which CH or SH combined with RelyX U100 were used showed higher bond strength values than RelyX ARC, regardless of the irrigant solution. There was no difference between the use of RelyX ARC after 7 and 180 days of storage. For Rely X U100 180 days of storage increased the push-out bond strength when either CH or SH was used. The dual-cure and self-adhesive resin cements associated with CH or SH demonstrated similar immediate bond strength performance. The self-adhesive cement, however, showed improved bond strength over time when either irrigant was used.     

Microtensile versus microshear bond strength between dental adhesives and the dentin substrate

This study evaluated the performance of different bonding tests on the bond strength of three adhesive systems to dentin. Forty-eight bovine incisors were used in the study, which were allocated in two groups according to the bond strength test performed: microtensile (µTBS) or microshear (µSBS). Also, each group was divided in three subgroups according to the adhesive system applied: Single Bond (SB), Prime & Bond (PB) and XP Bond (XPB) (n=8). The teeth were prepared according to each bond strength test protocol, and then the specimens were tested in an universal testing machine (EMIC). The data were submitted to two-way ANOVA (bond strength test and adhesive system type factors) and Tukey's post hoc test (α=0.05). The µTBS results were higher for all the adhesives when compared to the µSBS ones. Within the µTBS results, SB showed higher bond strength than PB and XPB, which showed similar adhesive performance among each other; within the µSBS results, all the adhesives presented similar bond strength values to dentin. The µTBS test detected differences between the adhesive systems evaluated; in contrast, the µSBS test was less discriminating in evaluating the adhesive performance of the materials tested.