Stability of the Dentin-Bonded Interface Using Self-Etching Adhesive Containing Diacrylamide after Bacterial Challenge.

Purpose/Aim: Acrylamides are hydrolytically stable at pH lower than 2, and were shown to preserve bonded interface integrity with two-step, total etch adhesives. The objective of this study was to leverage those two characteristics in self-etching primers containing the acidic monomer 10-MDP and test the microtensile bond strength before and after incubation with S. mutans incubation. Materials and Methods: Acidic primers (10 wt % 10-methacryloyloxydecyl dihydrogen phosphate─10-MDP; 45 wt % N,N-diethyl-1,3-bis(acrylamido)propane─DEBAAP, or 2-hydroxyethyl methacrylate─HEMA; 45 wt %, glycerol-dimethacrylate─GDMA) and adhesives (DEBAAP or HEMA/10-MDP/UDMA 45/10/45 wt %) were made polymerizable by the addition of 0.2 wt % camphorquinone, 0.8 wt % ethyl-4-dimethylaminobenzoate, 0.4 wt % diphenyliodonium hexafluorophosphate, and 0.1 wt % butylhydroxytoluene. Nonsolvated materials were characterized for flexural strength (FS), modulus (E), toughness, water sorption/solubility (WS/SL), contact angle, and vinyl conversion (DC). Viscosity was evaluated after adding 20 and 40 vol % ethanol to the primer and adhesive, respectively. The experimental materials or Clearfil SE Bond (CC─commercial control) were used to bond a commercial composite (Filtek Supreme) to the flat surface of human dentin. Microtensile bond strength (MTBS) was tested in 1 mm2 sticks for the 5 primer/bond combinations: CC (Clearfil Bond Primer and Bond), HH (HEMA/HEMA), DD (DEBAAP/DEBAAP), HD (HEMA/DEBAAP), and DH (DEBAAP/HEMA). Prior to testing, sticks were stored in water or biofilm-inducing culture medium with S. mutans for 1 week. Confocal images and FTIR-ATR evaluation evaluated the hybrid layer of the adhesives. Results were analyzed using Student's t-test (WS, SL, DC, contact angle, FS, E, toughness), one-way ANOVA/Tukey's test for viscosity, and two-way ANOVA/Tukey's test for MTBS (95%). Results: HEMA-based materials had lower contact angle (p = 0.004), higher WS (p < 0.001), and similar SL values compared to DEBAAP (p = 0.126). FS (p = 0.171) and E (p = 0.065) dry values were similar, but after one week of water storage, FS/E dropped more significantly for HEMA materials. Dry and wet toughness was greater for DEBAAP (p < 0.001), but it also had the greatest drop (46%). Clearfil bonds had the highest viscosity, followed by DEBAAP and HEMA, respectively (p = 0.002). For the primers, HEMA had the lowest viscosity (p = 0.003). As far as MTBS, all groups tested in water were statistically different when compared with HH (p < 0.001). After storage in biofilm, DH had the highest MTBS value, being statistically different from HH (p = 0.002), CC (p = 0.015), and DD (p = 0.027). Conclusions: The addition of a diacrylamide and its association with HEMA in self-etching adhesive systems provided greater bonding stability after bacterial challenge.

Effect of hydrofluoric acid concentration and aging on the bond strength ceramics to a resin cement.

This study evaluated the influence of hydrofluoric acid (HF) concentration and thermal cycling on the microshear bond strength (µSBS) of a resin luting agent to IPS e.max® CAD and Rosetta® SM. Ceramic specimens (12.0 x 14.0 x 1.5mm) were randomized into 8 groups (n=10) according to HF concentration, commercial brand, and aging. Immediately after polishing, and etching, all specimens were silanized and a layer of adhesive was applied. A PVS mold of 3 mm thickness and 10mm diameter with (four) 1.0mm holes was fabricated, placed on each specimen, and then filled with a resin luting agent. Half of the specimens were subjected to the µSBS test using an Instron at a speed of 1.0 mm/min, following a 24-hour storage in deionized water at 37ºC. The remaining specimens were subjected to thermal cycling (5ºC-55ºC, 30 seconds per bath) and µSBS. The data were evaluated utilizing a three-way ANOVA and Tukey's post-hoc test (α=0.05). Significant differences were found for HF concentration and aging (p<0.0001). No significant difference in µSBS was found for commercial brands (p=0.085). The interaction between brand and HF concentration (p=0.358), brand and aging (p=0.135), and HF concentration and aging (p=0.138) were not statistically significant. The triple interaction among these factors was not statistically significant (p=0.610). In conclusion, the bond strength is affected by the HF concentration. No statistical difference was observed between the two ceramics. Thermal cycling significantly reduced µSBS.

Cellulose acetate scaffold coated with a hydroxyapatite/graphene oxide nanocomposite for application in tissue engineering.

The objective of this study was to synthesize and characterize porous Cellulose Acetate (CA) scaffolds using the electrospinning technique and functionalize the surface of the scaffolds obtained through the dip-coating method with a Hydroxyapatite (HA) nanocomposite and varying concentrations of graphene oxide (GO) for application in tissue engineering regeneration techniques. The scaffolds were divided into four distinct groups based on their composition: 1) CA scaffolds; 2) CAHAC scaffolds; 3) CAHAGOC 1.0% scaffolds; 4) CAHAGOC 1.5% scaffolds. Scaffold analyses were conducted using X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Raman Spectroscopy, Scanning Electron Microscopy with Energy Dispersive Spectroscopy (SEM/EDS), and in vitro cell viability assays (WST). For the biological test analysis, Variance (two-way) was used, followed by Tukey's post-test (α = 0.05). The XRD results revealed the predominant presence of CaP phases in the CAHAC, CAHAGOC 1.0%, and CAHAGOC 1.5% groups, emphasizing the presence of HA in the scaffolds. FTIR demonstrated characteristics of cellulose and PO4 bands in the groups containing HA, confirming the presence of CaP in the synthesized materials, as also indicated by XRD. Raman spectroscopy showed the presence of D and G bands, consistent with GO, confirming the successful incorporation of the HAGO nanocomposite into the scaffolds. The micrographs displayed overlapping electrospun fibers, forming the three-dimensional structure in the produced scaffolds. It was possible to observe hydroxyapatite crystals filling some of these pores, creating a suitable structure for cell adhesion, proliferation, and nutrition, as corroborated by the results of in vitro tests. All scaffolds exhibited high cell viability, with significant cell proliferation. Even after 48 h, there was a slight reduction in the number of cells, but a noteworthy increase in cell proliferation was evident in the CAHAGOC 1.5% group after 48 h (p < 0.05). In conclusion, it can be affirmed that the produced scaffolds demonstrated physical and biological characteristics and properties capable of promoting cell adhesion and proliferation. Therefore, they represent significant potential for application in tissue engineering, offering a new perspective regarding techniques and biomaterials applied in regenerative therapies.

Multi-acrylamides improve bond stability through collagen reinforcement under physiological conditions.

OBJECTIVES: Acrylamides were shown to significantly improve bonding stability in adhesive restorations, but the reinforcement mechanism has not been fully elucidated. We tested the hypothesis that hydrogen bonding reinforcement of the collagen network (with secondary or tertiary acrylamides), as well as degree of crosslinking of the polymer network (with di- or tri-functional acrylamides), can be two of the factors at play. METHODS: Two-step total etch adhesives comprising UDMA (60 wt%) and 40 wt% of: TAAEA, TMAAEA (secondary, tertiary tri-acrylamides), BAAP, DEBAAP (secondary, tertiary di-acrylamides) or HEMA (mono-methacrylate - control) were formulated. Simulated composite restorations (n = 5) were tested after cyclic mechanical and biological (S. mutans biofilm) challenges. Gap formation before and after aging was assessed with SEM imaging. Micro-tensile bond strength (µTBS, n = 6) was assessed after seven-day incubation in water or S. mutans-containing culture medium. Collagen reinforcement was assessed with hydroxyproline assay (n = 10) and rheology (n = 3). Data were analyzed with one-way/two-way ANOVA/Tukey's test (alpha=5%). RESULTS: Gap formation increased and bond strength decreased for all monomers after biofilm incubation (p < 0.001). Except for DEBAAP, secondary and tertiary di/tri-acrylamides showed lower occlusal gap width values, but no significant differences overall gap length compared to HEMA. µTBS increased for tri-acrylamides compared with HEMA. Samples treated with multi-acrylamides had lower concentration of hydroxyproline (by-product of collagen degradation) (p < 0.001), except for DEBAAP, which showed values close to HEMA (p > 0.05). Dentin shear modulus increased for all acrylamides after 72 h, especially TMAAEA. SIGNIFICANCE: In general, multi-acrylamides promote collagen reinforcement, leading to reduced gap formation, and stabilize the bond strength under physiological conditions.

Surface treatments of the zirconia-reinforced lithium disilicate ceramic in the adhesion to the resin cement.

This study verified the effect of surface treatments of the zirconia-reinforced lithium disilicate ceramic bonded to resin cement. Ceramic blocks were divided according to treatments (n=10): FA+SRX (Fluoric acid + silane RX), FA+MDP (Fluoric acid + MDP), FA+SCF+MDP (Fluoric acid + silane CF + MDP), FA+MEP (Fluoric acid + MEP), and MEP (Self-etch primer). Resin cement cylinders were made in the ceramic blocks, photoactivated with 1,200 mW/cm² for 40s, stored in water at 37°C for 24h, and evaluated by the microshear strength test, optical failure descriptive analysis (%), surface characterization (SEM) and contact angle (Goniometer). Other samples were submitted to 10,000 thermocycles between 5°C and 55°C. Bond strength data were submitted to two-way ANOVA and Tukey's test. Contact angle to one-way ANOVA and Games-Howell's test (5%). At 24h, MEP showed higher bond strength, and FA+SRX the lower. FA+MDP and FA+SCF+MDP showed similar values and FA+MEP was intermediate. After thermocycling, FA+SCF+MDP, FA+MEP, and MEP showed higher values, and FA+SRX the lower while FA+MDP was intermediate. When the periods were compared, FA+MDP, FA+SCF+MDP, FA+MEP, and MEP showed higher values for 24h while FA+SRX was similar. SEM showed retentive surface and crystal exposure when treated with FA+SCF+MDP. The less retentive surface was obtained with MEP, and the other treatments promoted intermediate irregularities. In conclusion, surface treatment and thermocycling promoted different values of adhesive strength and contact angle in a zirconia-reinforced lithium silicate ceramic. Failures were predominantly adhesive, and the ceramic surface was characterized by different levels of roughness and selective exposure of crystals.

Effect of Ceramic Thickness on the Bond Strength to Resin-Luting Agents before and after Thermal Cycling.

This study investigated microshear bond strength (µSBS) of two (2) dual-cured resin-luting agents (RelyX™ Ultimate and RelyX™ U200) when photoactivated through varying thicknesses of lithium disilicate, with or without thermal cycling. Discs of IPS e.max Press of 0.5, 1.5, and 2 mm in thickness were obtained. Elastomer molds (3.0 mm in thickness) with four cylinder-shaped orifices 1.0 mm in diameter, were placed onto the ceramic surfaces and filled with resin-luting agents. A Mylar strip, glass plate, and load of 250 grams were placed over the filled mold. The load was removed and the resin-luting agents were photoactivated through the ceramics using a single-peak LED (Radii Plus.) All samples were stored in distilled water at 37oC for 24 h. Half of the samples were subjected to thermal cycling (3,000 cycles; 5ºC and 55ºC). All samples were then submitted to µSBS test using a universal testing machine (Instron 4411) at a crosshead speed of 0.5 mm/min. Data were submitted to three-way ANOVA and Tukey post-hoc test (α=0.05). The mean µSBS at 24 h was significantly higher than after thermal cycling (p<0.05). No statistical difference was found between resin-luting agents (p > 0.05). The mean µSBS for groups photoactivated through 0.5 mm ceramic were significantly higher than 1.5 mm and 2.0 mm (p < 0.05). In conclusion, increased ceramic thicknesses reduced the bond strength of tested resin-luting agents to lithium disilicate. No differences were found between resin-luting agents. Thermal cycling reduced the bond strength of both resin-luting agents.

Preheated acid associated with silane and electric current in the adhesion of the resin cement to ceramic.

This study verified the effect of the combination of preheated hydrofluoric acid/silane/electric current in the adhesion of the resin cement to ceramic. IPS E.max Press ceramic discs embedded in PVC rigid tubes were divided into four groups associating preheated hydrofluoric acid and silane applied with electrical current (n=10): Ha+S (Heated acid + silane); Ha+S+Ec (Heated acid + silane + electrical current); A+S (Acid + silane) and A+S+Ec (Acid + silano + electrical current). Resin cement/ceramic samples were stored in water at 37°C for 24h. After storage, they were submitted to the microshear test, fracture analysis, and contact angle at 24h or after thermocycling (10,000 cycles/5-55ºC). Bond strength data were evaluated by two-way ANOVA. For comparison between evaluation times (24h or thermocycling) was applied unpaired t-test. A significance post-hoc test of p=0.05 was assumed for analyses and graphs (GraphPad Prism 9.0 software). At 24h, the microshear strength showed similar values between Ha+S, Ha+S+Ec, and A+S+Ec groups, while A+S showed the lowest value with a statistical difference. After thermocycling, Ha+S and Ha+S+Ec were similar, as well as A+S and A+S+Ec. There was a significant difference in all groups comparing 24h (highest value) with after thermocycling (lowest value). Adhesive fracture was predominant in all groups and evaluation times. Ha+S and A+S groups showed higher contact angle values compared to the Ha+S+Ec and A+S+Ec with lower values. In conclusion, the association of preheated hydrofluoric acid/silane applied or not with electric current promoted different microshear strength values, fracture types, and contact angles in the resin cement/ceramic bond.

Evaluation of mechanical properties and morphology of miniscrews Ti6Al4V cold worked versus annealed in artificial bones.

PURPOSE: This study aimed to evaluate the influence of different manufacturing procedures (Eli annealed - hot work versus cold worked - cold work) of the raw material under mechanical properties and morphological characteristics of orthodontic miniscrews (MS). MATERIAL AND METHODS: Thirty MS were randomly separated into 3 types (n=10) according to manufacturer and manufacturing process of the raw material: type A - SIN® annealed (control group); type B - Dentfix® annealed; and, type C - Dentfix® cold worked. MI were inserted in artificial bone blocks, through the manufacturer's specific manual key attached to the digital torquemeter stabilized via custom device. Data of fracture's occurrence was performed using Fisher's exact test. Comparisons between the other two types regarding insertion torque and removal torque were performed using the Mann-Whitney test. Data of fracture torque, shear stress, normal stress and torque ratio was submitted to Kruskal Wallis and Dunn tests (α=0.05). Representative images of surface morphology and fractures were selected. RESULTS: Type C showed statistically the lowest fracture torque (N.cm) (26.11±0.41) (P=0.0012) and highest torque ratio (%) (98.74±0.85) (P=0.0007). Type C showed statistically higher calculated shear (MPa) (2,432.73±508.41) and normal stress (MPa) (1,403.86±293.39) than type B and type A, showing that they differed in relation to the mechanical strength of the material with which they were made (P=0.0007). CONCLUSION: Type A fractured completely inside the most apical bone. Type B and type C fractured closer to the transmucosal profile. Cold worked process should be more prone to fractures than those annealed raw manufactured.

Preheated acid associated with silane and electric current in the adhesion of the resin cement to ceramic

Abstract This study verified the effect of the combination of preheated hydrofluoric acid/silane/electric current in the adhesion of the resin cement to ceramic. IPS E.max Press ceramic discs embedded in PVC rigid tubes were divided into four groups associating preheated hydrofluoric acid and silane applied with electrical current (n=10): Ha+S (Heated acid + silane); Ha+S+Ec (Heated acid + silane + electrical current); A+S (Acid + silane) and A+S+Ec (Acid + silano + electrical current). Resin cement/ceramic samples were stored in water at 37°C for 24h. After storage, they were submitted to the microshear test, fracture analysis, and contact angle at 24h or after thermocycling (10,000 cycles/5-55ºC). Bond strength data were evaluated by two-way ANOVA. For comparison between evaluation times (24h or thermocycling) was applied unpaired t-test. A significance post-hoc test of p=0.05 was assumed for analyses and graphs (GraphPad Prism 9.0 software). At 24h, the microshear strength showed similar values between Ha+S, Ha+S+Ec, and A+S+Ec groups, while A+S showed the lowest value with a statistical difference. After thermocycling, Ha+S and Ha+S+Ec were similar, as well as A+S and A+S+Ec. There was a significant difference in all groups comparing 24h (highest value) with after thermocycling (lowest value). Adhesive fracture was predominant in all groups and evaluation times. Ha+S and A+S groups showed higher contact angle values compared to the Ha+S+Ec and A+S+Ec with lower values. In conclusion, the association of preheated hydrofluoric acid/silane applied or not with electric current promoted different microshear strength values, fracture types, and contact angles in the resin cement/ceramic bond.

Resumo Este estudo verificou o efeito da combinação ácido fluorídrico pré-aquecido/silano/corrente elétrica na adesão do cimento resinoso à cerâmica. Os discos cerâmicos IPS E.max Press embutidos em tubos rígidos de PVC foram separados em quatro grupos associando ácido fluorídrico pré-aquecido e silano aplicado com corrente elétrica (n=10): Ha+S (ácido aquecido + silano); Ha+S+Ec (Ácido aquecido + silano + corrente elétrica); A+S (Ácido + silano) e A+S+EC (Ácido + silano + corrente elétrica). Amostras de cimento resinoso/cerâmica foram armazenadas em água a 37°C por 24 horas. Após o armazenamento foram submetidas ao ensaio de micro cisalhamento, análise de fratura e ângulo de contato no período de 24 horas ou após termociclagem (10.000 ciclos/5-55ºC). Os dados de resistência de união foram avaliados por ANOVA dois fatores. Para comparação entre os tempos de avaliação (24 horas ou termociclagem) foi aplicado o teste t não pareado. Foi assumida significância de 5% para análises e gráficos (software GraphPad Prism 9.0). Em 24 horas, a resistência ao micro cisalhamento apresentou valores similares entre os grupos Ha+S, Ha+S+Ec e A+S+Ec, enquanto A+S apresentou menor valor com diferença estatística. Após a termociclagem, Ha+S e Ha+S+Ec foram similares, assim como A+S e A+S+Ec. Houve diferença significativa em todos os grupos comparando 24 horas (maior valor) com após termociclagem (menor valor). A fratura adesiva foi predominante em todos os grupos e tempos de avaliação. Os grupos Ha+S e A+S apresentaram maiores valores de ângulos de contato comparados aos grupos Ha+S+Ec e A+S+Ec com valores menores. Em conclusão, a associação ácido fluorídrico pré-aquecido/silano aplicado com corrente elétrica promoveu diferentes valores de resistência ao micro cisalhamento, tipos de fratura e ângulos de contato na adesão do cimento resinoso à cerâmica.

Effect of Ceramic Thickness on the Bond Strength to Resin-Luting Agents before and after Thermal Cycling

Abstract This study investigated microshear bond strength (µSBS) of two (2) dual-cured resin-luting agents (RelyX™ Ultimate and RelyX™ U200) when photoactivated through varying thicknesses of lithium disilicate, with or without thermal cycling. Discs of IPS e.max Press of 0.5, 1.5, and 2 mm in thickness were obtained. Elastomer molds (3.0 mm in thickness) with four cylinder-shaped orifices 1.0 mm in diameter, were placed onto the ceramic surfaces and filled with resin-luting agents. A Mylar strip, glass plate, and load of 250 grams were placed over the filled mold. The load was removed and the resin-luting agents were photoactivated through the ceramics using a single-peak LED (Radii Plus.) All samples were stored in distilled water at 37oC for 24 h. Half of the samples were subjected to thermal cycling (3,000 cycles; 5ºC and 55ºC). All samples were then submitted to µSBS test using a universal testing machine (Instron 4411) at a crosshead speed of 0.5 mm/min. Data were submitted to three-way ANOVA and Tukey post-hoc test (α=0.05). The mean µSBS at 24 h was significantly higher than after thermal cycling (p<0.05). No statistical difference was found between resin-luting agents (p > 0.05). The mean µSBS for groups photoactivated through 0.5 mm ceramic were significantly higher than 1.5 mm and 2.0 mm (p < 0.05). In conclusion, increased ceramic thicknesses reduced the bond strength of tested resin-luting agents to lithium disilicate. No differences were found between resin-luting agents. Thermal cycling reduced the bond strength of both resin-luting agents.

Resumo: Este estudo investigou a resistência de união ao microcisalhamento (RUµC) de dois (2) agentes de cimentação de resina dual (RelyX™ Ultimate e RelyX™ U200) quando fotoativados através de diferentes espessuras de dissilicato de lítio, com ou sem ciclagem térmica. Discos do IPS e.max Press de 0,5, 1,5 e 2 mm de espessura foram obtidos. Moldes de elastômero (3,0 mm de espessura) com quatro orifícios cilíndricos de 1,0 mm de diâmetro foram colocados sobre as superfícies cerâmicas e preenchidos com agentes de cimentação de resina. Uma tira Mylar, placa de vidro e carga de 250 gramas foram colocadas sobre o molde preenchido. A carga foi removida e os agentes de cimentação resinosos foram fotoativados através da cerâmica usando um LED de pico-único (Radii Plus). Todas as amostras foram armazenadas em água deionizada a 37oC por 24 h. Metade das amostras foi submetida a ciclagem térmica (3.000 ciclos; 5ºC e 55ºC). Todas as amostras foram então submetidas ao teste de RUµC usando uma máquina de teste universal (Instron 4411) com velocidade de 0,5 mm/min. Os dados foram submetidos à Análise de Variância três fatores e ao teste post-hoc de Tukey (α = 0,05). A média de RUµC em 24 h foi significativamente maior do que após a ciclagem térmica (p < 0,05). Não houve diferença estatística entre os cimentos resinosos (p > 0,05). As médias de RUµC para grupos fotoativados através de cerâmica de 0,5 mm foram significativamente maiores do que 1,5 mm e 2,0 mm (p < 0,05). Em conclusão, o aumento da espessura da cerâmica reduziu a resistência de união dos agentes de cimentação resinosos ao dissilicato de lítio. Não foram encontradas diferenças entre os agentes de cimentação resinosos. A ciclagem térmica reduziu a resistência de união de ambos os agentes de cimentação resinosos.

Surface treatments of the zirconia-reinforced lithium disilicate ceramic in the adhesion to the resin cement

Abstract This study verified the effect of surface treatments of the zirconia-reinforced lithium disilicate ceramic bonded to resin cement. Ceramic blocks were divided according to treatments (n=10): FA+SRX (Fluoric acid + silane RX), FA+MDP (Fluoric acid + MDP), FA+SCF+MDP (Fluoric acid + silane CF + MDP), FA+MEP (Fluoric acid + MEP), and MEP (Self-etch primer). Resin cement cylinders were made in the ceramic blocks, photoactivated with 1,200 mW/cm² for 40s, stored in water at 37°C for 24h, and evaluated by the microshear strength test, optical failure descriptive analysis (%), surface characterization (SEM) and contact angle (Goniometer). Other samples were submitted to 10,000 thermocycles between 5°C and 55°C. Bond strength data were submitted to two-way ANOVA and Tukey's test. Contact angle to one-way ANOVA and Games-Howell's test (5%). At 24h, MEP showed higher bond strength, and FA+SRX the lower. FA+MDP and FA+SCF+MDP showed similar values and FA+MEP was intermediate. After thermocycling, FA+SCF+MDP, FA+MEP, and MEP showed higher values, and FA+SRX the lower while FA+MDP was intermediate. When the periods were compared, FA+MDP, FA+SCF+MDP, FA+MEP, and MEP showed higher values for 24h while FA+SRX was similar. SEM showed retentive surface and crystal exposure when treated with FA+SCF+MDP. The less retentive surface was obtained with MEP, and the other treatments promoted intermediate irregularities. In conclusion, surface treatment and thermocycling promoted different values of adhesive strength and contact angle in a zirconia-reinforced lithium silicate ceramic. Failures were predominantly adhesive, and the ceramic surface was characterized by different levels of roughness and selective exposure of crystals.

Resumo O objetivo neste estudo foi verificar o efeito de tratamentos de superfície da cerâmica de dissilicato de lítio reforçada com zircônia fixada ao cimento resinoso. Os blocos cerâmicos foram separados de acordo com os tratamentos (n=10): AF+SRX (ácido fluorídrico + silano), AF+MDP (ácido fluorídrico + MDP), AF+SCF+MDP (ácido fluorídrico + silano + MDP), AF+MEP (Ácido fluorídrico + MEP) e MEP (Primer auto condicionante). Cilindros de cimento resinoso foram confeccionados em cada bloco cerâmico, foto ativados com 1.200 mW/cm² por 40 segundos, armazenados em água a 37°C por 24 horas e avaliados pelo teste de resistência ao micro cisalhamento, falha por análise descritiva em microscopia óptica (%), caracterização da superfície por imagens MEV e ângulo de contato (Goniômetro). Outras amostras foram submetidas a 10.000 ciclos térmicos (5° e 55°C). Os dados de resistência de união foram submetidos a ANOVA dois fatores e teste de Tukey (5%). Ângulo de contato com ANOVA um fator e teste de Games-Howell (5%). Em 24 horas, MEP apresentou maior resistência de união e AF+S a menor. AF+MDP e AF+SCF+MDP apresentaram valores similares e AF+MEP foi intermediário. Após a ciclagem térmica, AF+SCF+MDP, AF+MEP e MEP apresentaram valores maiores e AF+SRX o menor enquanto AF+MDP foi intermediário. Quando comparados os períodos, AF+MDP, AF+SCF+MDP, AF+MEP e MEP apresentaram valores maiores em 24 horas enquanto AF+SRX foi similar. MEV mostrou superfície mais retentiva e exposição de cristais quando tratada com AF+SCF+MDP. A superfície menos retentiva foi obtida com MEP, e os demais tratamentos promoveram irregularidades de superfície intermediárias. Conclui-se que o tratamento superficial e a termociclagem promoveram diferentes valores de resistência adesiva e ângulo de contato em cerâmica de silicato de lítio reforçada com zircônia. As falhas foram predominantemente adesivas, e a superfície cerâmica foi caracterizada com diferentes níveis de rugosidade e exposição seletiva de cristais.

Effect of hydrofluoric acid concentration and aging on the bond strength ceramics to a resin cement

Abstract This study evaluated the influence of hydrofluoric acid (HF) concentration and thermal cycling on the microshear bond strength (µSBS) of a resin luting agent to IPS e.max® CAD and Rosetta® SM. Ceramic specimens (12.0 x 14.0 x 1.5mm) were randomized into 8 groups (n=10) according to HF concentration, commercial brand, and aging. Immediately after polishing, and etching, all specimens were silanized and a layer of adhesive was applied. A PVS mold of 3 mm thickness and 10mm diameter with (four) 1.0mm holes was fabricated, placed on each specimen, and then filled with a resin luting agent. Half of the specimens were subjected to the µSBS test using an Instron at a speed of 1.0 mm/min, following a 24-hour storage in deionized water at 37ºC. The remaining specimens were subjected to thermal cycling (5ºC-55ºC, 30 seconds per bath) and µSBS. The data were evaluated utilizing a three-way ANOVA and Tukey's post-hoc test (α=0.05). Significant differences were found for HF concentration and aging (p<0.0001). No significant difference in µSBS was found for commercial brands (p=0.085). The interaction between brand and HF concentration (p=0.358), brand and aging (p=0.135), and HF concentration and aging (p=0.138) were not statistically significant. The triple interaction among these factors was not statistically significant (p=0.610). In conclusion, the bond strength is affected by the HF concentration. No statistical difference was observed between the two ceramics. Thermal cycling significantly reduced µSBS.

Resumo Este estudo avaliou a influência da concentração do ácido fluorídrico (AF) e da ciclagem térmica na resistência de união ao microcisalhamento (RUµC) de um cimento resinoso para IPS e.max® CAD e Rosetta® SM. Espécimes cerâmicos (12,0 x 14,0 x 1,5mm) foram divididos em 8 grupos (n=10) de acordo com concentração do HF, marca comercial e envelhecimento. Imediatamente após o polimento e condicionamento ácido, todos os espécimes foram silanizados e uma camada de adesivo foi aplicada. Um molde PVS de 3 mm de espessura e 10 mm de diâmetro com (quatro) orifícios de 1,0 mm foi confeccionado, colocado em cada espécime e preenchido com o cimento resinoso. Metade dos espécimes foi submetida ao teste RUµC na Instron a velocidade de 1,0 mm/min, após 24 horas de armazenamento em água deionizada a 37ºC. Os espécimes restantes foram submetidos a ciclagem térmica (5ºC-55ºC, 30 segundos por banho) e a RUµC. Os dados foram avaliados por ANOVA de três fatores e ao teste post-hoc de Tukey (α=0,05). Diferenças significativas foram encontradas para concentração de HF e envelhecimento (p<0,0001). Nenhuma diferença significativa na RUµC foi encontrada para cada marca comercial (p=0,085). A interação entre marca comercial e a concentração do HF (p=0,358), marca comercial e envelhecimento (p=0,135) e concentração do HF e envelhecimento (p=0,138) não foram estatisticamente significativas. A tripla interação entre esses fatores não foi estatisticamente significativa (p=0,610). Concluindo, a resistência de união é afetada pela concentração de HF. Não foi observada diferença estatística entre as duas cerâmicas. A ciclagem térmica reduziu significativamente a resistência de união ao microcisalhamento.

Deflection of tandem archwire in a specific self-ligating metal bracket system: an in vitro study.

The aim of this study was to quantify the force exerted by tandem archwires in a specific system of passive self-ligating bracket. Forty-eight thermo-activated nickel-titanium orthodontic archwires were separated into four groups (n = 12): G1 - two .014" + .014" round archwires; G2 - two .014" + .016" round archwires; G3 - .014" x .025" rectangular archwire; and. G4 - .016" x .022" rectangular archwire. Brackets were fixed onto teeth 1.5 to 2.5 using a device that represented the upper teeth, maintaining an interbracket distance of 6.0 mm. The deflection tests were performed using the structure representative of tooth 1.1 as support on the Instron testing machine at a speed of 2.0 mm/min. The archwires were evaluated at deflections of 0.5 mm, 1.0 mm, and 1.5 mm. The data were analyzed by a generalized linear model, considering values at different deflections as repeated measurements in the same experimental unit (α = 0.5%). At 0.5 mm, higher forces were observed in G2 and G3, which did not differ significantly (p > 0.05). The lowest force was observed in G4 (p < 0.05). At 1.0 mm and 1.5 mm, the highest force was observed in G3, followed by G4 and G2 (p < 0.05). The lowest force was observed in G1 (p < 0.05). In general, tandem archwires (same or different calibers) in a specific passive self-ligating bracket exerted lower force when compared with rectangular archwires.

Curing profile and marginal gap formation using a liner containing long-wavelength-absorbing photoinitiator: an in vitro study.

The aim was to evaluate the marginal-gap formation and curing profile of a new restorative technique using a liner with long-wavelength-absorbing photoinitiator (LWAP). Box-shaped preparations (6 mm × 4 mm × 4 mm) were made in third molars. All samples were treated with Clearfill SE Bond and divided into 4 groups (n = 5), according to restorative technique used: (1) incremental technique (INC-Technique); (2) camphorquinone-based liner (CQ-Liner) + bulk-fill resin composite; (3) LWAP-based liner (LWAP-Liner) + bulk-fill resin composite; and (4) bulk-fill technique without liner (BF-Technique). The marginal gaps (%) for all the samples were measured using micro-computed tomography. The restorations were cross-sectioned, and the degree of conversion (DC) and Knoop microhardness were evaluated at different depths (0.3, 1, 2, 3, and 4 mm). INC-Technique, CQ-Liner, and LWAP-Liner groups showed significantly fewer marginal gaps than those from the BF-Technique group. The BF-Technique specimens had the lowest DC and microhardness in depth. All the other techniques presented similar degree of conversion and microhardness at all the depths. The use of liners, regardless of the photoinitiator system, decreased the marginal-gap formation and improved the curing profile of bulk-filling restoration technique.

Chitosan/Xanthan/Hydroxyapatite-graphene oxide porous scaffold associated with mesenchymal stem cells for dentin-pulp complex regeneration.

The aim of this paper was to synthesize and characterize polymeric scaffolds of Chitosan/Xanthan/Hydroxyapatite-Graphene Oxide nanocomposite associated with mesenchymal stem cells for regenerative dentistry application. The chitosan-xanthan gum (CX) complex was associated with Hydroxyapatite-Graphene Oxide (HA-GO) nanocomposite with different Graphene Oxides (GO) concentration (0.5 wt%; 1.0 wt%; 1.5 wt%). The scaffolds characterizations were performed by X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Raman spectroscopy, thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and contact angle. The mechanical properties were assessed by compressive strength. The in vitro bioactivity and the in vitro cytotoxicity test (MTT test) were analyzed as well. The data was submitted to the Normality and Homogeneity tests. In vitro Indirect Cytotoxicity assay data was statistically analyzed by ANOVA two-way, followed by Tukey's test (α = 0.05). Compressive strength and contact angle data were statistically analyzed by one-way ANOVA, followed by Tukey's test (α = 0.05). XRD showed the presence of Hydroxyapatite (HA) peaks in the structures CXHA, CXHAGO 0.5%,1.0% and 1.5%. FT-IR showed amino and carboxylic bands characteristic of CX. Raman spectroscopy analysis evidenced a high quality of the GO. In the TGA it was observed the mass loss associated with the CX degradation by depolymerization. SEM analysis showed pores in the scaffolds, in addition to HA incorporated and adhered to the polymer. Contact angle test showed that scaffolds have a hydrophilic characteristic, with the CX group the highest contact angle and CXHA the lowest (p < 0.05). 1.0 wt% GO significantly increased the compressive strength compared to other compositions. In the bioactivity test, the apatite crystals precipitation on the scaffold surface was observed. MTT test showed high cell viability in CXHAGO 1.0% and CXHAGO 1.5% scaffold. CXHAGO scaffolds are promising for regenerative dentistry application because they have morphological characteristics, mechanical and biological properties favorable for the regeneration process.

Delayed light-curing of dual-cure bulk-fill composites on internal adaptation and depth of cure.

OBJECTIVE: To evaluate the effect of delayed light-curing of dual-cure bulk-fill composites on internal adaptation and microhardness (KHN) in depth. MATERIALS AND METHODS: Bulk-fill composites were placed in 35 box-shaped preparations and cured according to the following protocols (n = 5): Filtek Bulk-Fill light-cured immediately after insertion (FBF); Bulk-EZ light-cured immediately after insertion (BEZ-I); Bulk-EZ light-cured 90 s after insertion (BEZ-DP); Bulk-EZ self-cured (BEZ-SC); HyperFIL light-cured immediately after insertion (HF-I); HyperFIL light-cured 90 s after insertion (HF-DP); HyperFIL self-cured (HF-SC). After 24 h, the samples were axially sectioned, and the internal adaptation was evaluated using replicas under a scanning electron microscope. The KHN was evaluated at six depths (0.3 mm, 1 mm, 2 mm, 3 mm, 4 mm, and 5 mm). The statistical analysis was performed using α = 0.05. RESULTS: The KHN significantly decreased with depth, except in self-curing mode, when it was similar at all depths. Delayed light-curing significantly increased the KHN at higher depths. The internal adaptation was material-dependent. Light-curing did not influence the internal adaptation of HyperFIL, whereas delayed light-curing significantly reduced the internal gaps (%) of Bulk-EZ. CONCLUSION: Delayed light-curing improved the depth of cure of dual-cure resin composites. Light-curing did not influence the internal adaptation of HyperFIL, but delayed light-curing improved the internal adaptation of Bulk-EZ. CLINICAL SIGNIFICANCE: Light-curing is fundamental for improving the mechanical properties of dual-cure resin composites. Moreover, depending on the dual-cure resin composite, the delay in light-curing can reduce the internal gaps.

Do cone-beam computed tomography low-dose protocols affect the evaluation of the temporomandibular joint?

BACKGROUND: There is no established acquisition protocol based on scientific evidence for the acquisition of cone-beam computed tomography (CBCT) exams to evaluate the temporomandibular joint (TMJ). OBJECTIVES: To evaluate the influence of acquisition protocols and jaw positioning on the diagnostic accuracy of TMJ condylar morphological alterations (CMA), dimension, position and excursion. METHODS: Thirty-six TMJs on 18 dry skulls were imaged using a CBCT unit (OP300 Maxio, Instrumentarium, Tuusula, Finland) at two exposure settings (4.5 and 6.3 mA), three voxel resolutions (0.085, 0.125 and 0.280 mm), three jaw positions (concentric, anteriorised and posteriorised) and three jaw excursions (normoexcursion, hyperexcursion and hypoexcursion). The macroscopic anatomy examination and high-resolution CBCT images were used as ground truth for CMA. Twenty-five TMJs had at least one CMA with 11 healthy TMJs serving as controls. Three experienced oral and maxillofacial radiologists evaluated the parasagittal images for the presence of CMA, position and excursion and measured dimensions. The area under the ROC curve, sensitivity and specificity were calculated. Weighted Kappa (α = 0.05) was used to determine intra- and interexaminer reliability and comparisons between dependent variables analysed by Analysis of Variance at an a prior level of significance of 0.05. RESULTS: The agreement of the evaluation of the position and excursion with the reference standard was high, independent of the protocol (range, 0.75-0.91). Various combinations of acquisition protocols and jaw position did not influence the CMA evaluation. Erosion was overdiagnosed in protocols with larger voxel sizes and the detection of osteophytes greater in images with smaller voxel sizes. The anteroposterior dimension was greater in the open jaw position (p < .05). CONCLUSION: CBCT protocols using reduced radiation exposure from the CBCT machine evaluated in this study can be used to assess condylar morphology, dimension, position and excursion, without compromising diagnostic performances for these parameters.

Deflection of tandem archwire in a specific self-ligating metal bracket system: an in vitro study

Abstract The aim of this study was to quantify the force exerted by tandem archwires in a specific system of passive self-ligating bracket. Forty-eight thermo-activated nickel-titanium orthodontic archwires were separated into four groups (n = 12): G1 - two .014" + .014" round archwires; G2 - two .014" + .016" round archwires; G3 - .014" x .025" rectangular archwire; and. G4 - .016" x .022" rectangular archwire. Brackets were fixed onto teeth 1.5 to 2.5 using a device that represented the upper teeth, maintaining an interbracket distance of 6.0 mm. The deflection tests were performed using the structure representative of tooth 1.1 as support on the Instron testing machine at a speed of 2.0 mm/min. The archwires were evaluated at deflections of 0.5 mm, 1.0 mm, and 1.5 mm. The data were analyzed by a generalized linear model, considering values at different deflections as repeated measurements in the same experimental unit (α = 0.5%). At 0.5 mm, higher forces were observed in G2 and G3, which did not differ significantly (p > 0.05). The lowest force was observed in G4 (p < 0.05). At 1.0 mm and 1.5 mm, the highest force was observed in G3, followed by G4 and G2 (p < 0.05). The lowest force was observed in G1 (p < 0.05). In general, tandem archwires (same or different calibers) in a specific passive self-ligating bracket exerted lower force when compared with rectangular archwires.

Chitosan/Xanthan membrane containing hydroxyapatite/Graphene oxide nanocomposite for guided bone regeneration.

OBJECTIVE: To develop a chitosan-xanthan (CX) membrane associated with Hydroxyapatite (HA) and different concentrations of graphene oxide (GO). METHODOLOGY: The CX complex was associated with the hydroxyapatite-graphene oxide (HAGO) nanocomposite in different concentrations. The experimental groups were:1) CX; 2) Chitosan-Xanthan/Hydroxyapatite (CXHA); 3) Chitosan-Xanthan/Hydroxyapatite-Graphene Oxide 0.5% (CXHAGO 0.5%); 4) CXHAGO 1.0%; 5) CXHAGO 1.5%. The membranes characterizations were performed by X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Raman spectroscopy, Scanning Electron Microscopy (SEM), Contact angle, Tensile Strength, in vitro Bioactivity and the in vitro Cell viability (MTT test). The data was submitted to the Normality and Homogeneity tests. In vitro Indirect Cytotoxicity assay data was statistically analyzed by two-way ANOVA and Tukey's test (α = 0.05). Tensile Strength and Contact Angle data were statistically analyzed by one-way ANOVA followed by Tukey's test (α = 0.05). RESULTS: XRD, FTIR and Raman spectroscopy confirmed the characteristic bands of the CX polymeric complex, the phosphate bands related to HA, and the presence of GO. SEM images demonstrated the non-porous and homogeneous surface of membranes. The contact angle test showed the hydrophilic characteristic of all membranes (p > 0.05). CX showed tensile strength significantly higher than other membranes. The apatite deposition was observed in all membranes after performing the bioactivity test. The cell viability of CXHAGO 1.0% and CXHAGO 1.5% was significantly higher than CX. CONCLUSION: The addition of HAGO reduced the mechanical strength of membranes, but improved its cell viability. It demonstrated the potential of CXHAGO membranes to be used in guided bone regeneration therapies.

Effect of horizontal slot of maxillary canines' brackets with varying wire angulations - An in vitro study.

A new device was developed to enable the visualization and measurement of canine angulation while at the same time visualizing and measuring the force transmitted to adjacent teeth. This study aimed to evaluate the mesiodistal tilt angle of the upper canine brackets, the wire deflection, and its effects on adjacent teeth with five different slot designs of upper canines. Wires (0.020" and 0.019" x 0.025") were tested on different five bracket types at five different distal angles. The force applied to adjacent teeth was measured as the angle was increased, and its consequences were observed in the posterior and anterior regions as well. The force tension (gf) was measured in a universal testing machine. Data were submitted to a 3-way ANOVA and Tukey's test (α=0.05). For both arches, regardless of the type of tooth and bracket type, the highest means tension mean values were shown by the 20° angle, followed by the 15°,10°, and 5° angles, which differed statistically among themselves. Overall, for 5°, 10°, and 15° angles, conventional and versatile brackets showed significantly higher force values in all teeth, tip-edge and control brackets showed the lowest. The highest force values were observed in central and lateral incisors with conventional and versatile brackets and on first and second premolar teeth with self-ligating passive and control brackets. Conventional brackets presented the highest forces, tip-edge and control brackets showed the lowest. The teeth that suffered the greatest forces were lateral incisors, and those that suffered the least were second premolars.