Cyclic Fatigue Resistance and Surface Roughness of Rotary NiTi Instruments after Simulated Clinical Use in Curved Root Canals - An Atomic Force Microscopy Study

Abstract Objective: To examine the cyclic fatigue resistance and surface topography of TruNatomy and ProTaper Gold nickel-titanium rotary files and evaluate the presence of alterations to surface topography following instrumentation in simulated curved canals. Material and Methods: Twenty-four nickel-titanium instruments, twelve each of TN and PTG file systems, were evaluated for cyclic fatigue resistance. The rotary files were rotated in a simulated root canal with standardized diameter, angle of curvature, and radius of curvature in a custom-made cyclic fatigue testing device until the instrument fracture occurred. The time to fracture for each instrument was recorded with a stopwatch; in seconds in each group. Fractured instruments were subjected to atomic force microscopy analysis measuring the average roughness and the root mean square values to investigate surface features of endodontic files. Mean values and standard deviation were calculated. Data were analyzed using the Mann-Whitney U test. Results: Time to fracture was marginally higher in PTG instruments than in the TN file systems. PTG files exhibited higher surface roughness when compared with TN files (p<0.05). Conclusion: TN file system had a higher cyclic fatigue resistance than PTG. Cyclic fatigue causing file breakage did affect the surface topography of the files. PTG files showed a higher surface porosity value than the TN files (AU).

Microscopic morphology observation of fracture healing process promoted by panax notoginseng saponins / Observación microscópica de la morfología del proceso de curación de fracturas promovida por panax notoginseng saponins

SUMMARY: The aim of this study was to explore promoting effect of external applying Panax Notoginseng Saponins (PNS) on fractures. For this analysis 18 New Zealand male rabbits were divided into control group, splintage group and PNS group. All rabbits were performed left radius fractures and natural healing, splintage healing and splintage coated with PNS healing. 2 rabbits in each group were sacrificed on day 14, day 28 and day 42 after surgery, separately. Atomic force microscope scanning and nanoindentation tests were performed on the callus sections. The particle size and roughness in PNS group was both less than that in splintage group. The elastic modulus of callus in PNS group was consistent with normal bone tissue started from day 28 after surgery, two weeks earlier than that in splintage group. PNS could significantly reduce fracture healing time and increase strength of callus.

RESUMEN: El objetivo de este estudio fue evaluar el efecto de la aplicación externa de Panax Notoginseng Saponins (PNS) en fracturas óseas. Se usaron 18 conejos machos de raza Nueva Zelanda divididos en grupos control, entablillado y PNS. Se realizaron fracturas del radio izquierdo y cicatrización natural en todos los animales, además de la cicatrización con entablillado y entablillado recubierto con PNS. Se sacrificaron, posterior a la cirugía, dos conejos de cada grupo los día 14, 28 y 42. Se realizaron pruebas de escaneo con microscopio de fuerza atómica y nanoindentación en las secciones de callos. El tamaño de la partícula y la rugosidad en el grupo de PNS fue menor que en el grupo entablillado. El módulo elástico del callo en el grupo de PNS fue consistente con el tejido óseo normal iniciado el día 28 después de la cirugía, dos semanas antes que en el grupo de entablillado. El PNS podría redu- cir significativamente el tiempo de curación de la fractura y aumentar la fuerza del callo.

Comparative Evaluation of Surface Roughness of Resin- Modified Glass Ionomer and Glass Hybrid Restorative Materials Simulated by Tooth Brushing: An in-Vitro Study

ABSTRACT Objective: Tocompare the effect of tooth brushing on surface roughness of Resin-Modified Glass Ionomer Cement (RMGIC; GC Gold label 2LC Light Cured Universal Restorative) and Glass Hybrid (GH; GC EQUIA SYSTEM- EQUIA Forte™ Fil and EQUIA Forte™ Coat) restorative material at 1- and 3-months interval simulated by tooth brushing. Material and Methods: RMGIC and GH material specimens (20 each) were prepared according to manufacturer instructions in 10mm × 2 mm dimensions using a mylar strip. A specially designed toothbrush simulator was used along with Oral B Pro 2 2000N powered toothbrush and Colgate Total dentifrice (Colgate-Palmolive India limited; Relative dentin abrasivity - RDA:70- Low abrasive) to perform brushing strokes. Specimens were subjected to surface roughness analysis before and after simulated tooth brushing at baseline, 1, and 3 months. Results: The intragroup comparison was done using repeated-measures ANOVA. Intergroup comparisons were done using an independent sample t-test and General Linear Model (ANCOVA). Surface roughness increased from baseline through 3 months in both RMGIC and GH groups. The mean surface roughness in RMGIC group was significantly higher than GH group at baseline 1 and 3-months, respectively (p<0.001, <0.001, and <0.001). Interaction between group and baseline surface roughness was not significant (p=0.466). The estimated marginal means were significantly higher in RMGIC than GH group (p=0.008). Conclusion: The surface roughness of both RMGIC and GH restorative increased from baseline to 1 month and 3 months after the simulated toothbrushing protocol. GH exhibited significantly lower surface roughness than RMGIC at all the tested intervals.

Applications of atomic force microscopy in immunology / 医学前沿

Cellular mechanics, a major regulating factor of cellular architecture and biological functions, responds to intrinsic stresses and extrinsic forces exerted by other cells and the extracellular matrix in the microenvironment. Cellular mechanics also acts as a fundamental mediator in complicated immune responses, such as cell migration, immune cell activation, and pathogen clearance. The principle of atomic force microscopy (AFM) and its three running modes are introduced for the mechanical characterization of living cells. The peak force tapping mode provides the most delicate and desirable virtues to collect high-resolution images of morphology and force curves. For a concrete description of AFM capabilities, three AFM applications are discussed. These applications include the dynamic progress of a neutrophil-extracellular-trap release by neutrophils, the immunological functions of macrophages, and the membrane pore formation mediated by perforin, streptolysin O, gasdermin D, or membrane attack complex.

Nanopartículas de clorexidina-hexametafosfato na endodontia: síntese, caracterização, avaliação biológica e físico-química da incorporação aos cimentos endodônticos / Chlorhexidine hexametaphosphate nanoparticles in endodontics: synthesis, characterization, biological and physicochemical evaluation of incorporation to endodontic sealers

Este estudo avaliou as influências da incorporação de nanopartículas (NPs) de clorexidina-hexametafosfato em diversas propriedades dos cimentos endodônticos: AH Plus, MTA Fillapex e Pulp Canal Sealer (PCS). As NPs foram sintetizadas através de uma suspensão contendo 5 mM de hexametafosfato de sódio (HMP) e 4 mM de digluconato de clorexidina (CHX) a 20%, caracterizadas por microscopia eletrônica de varredura (MEV), espalhamento dinâmico de luz (DLS), potencial zeta, microscopia de força atômica (AFM) e espectroscopia de energia dispersiva de raios-X (EDS). Os cimentos endodônticos sofreram incorporação, em peso, de 2% e 5% das NPs. A ação antimicrobiana das amostras foi avaliada pelo teste de difusão em ágar e contato direto (DCT) frente a Enterococcus faecalis. O DCT foi conduzido em 3 tempos de armazenamento: cimentos frescos (T0), após 7 dias (T7) e após 30 dias (T30), e nos tempos de contato: 10 e 60 min. A citotoxicidade foi avaliada conforme as normas ISO 10993-12 através de extratos preparados em meio de cultura Dulbecco's modified Eagle's medium. As interações dos fibroblastos da linhagem MRC-5 com as diluições seriadas (1:1 a 1:8) dos extratos foram analisadas através do ensaio de quantificação do metabolismo mitocondrial pelo tetrazollium (MTT). O escoamento, radiopacidade, solubilidade e tempo de presa das amostras foi avaliado segundo a norma ISO 6876:2012. A solubilidade foi avaliada após 24 horas e 7 dias de imersão das amostras e o pH aferido após: 3h, 24h, 48h, 72h e 7 dias de armazenamento. Os resultados obtidos foram submetidos à análise estatística por análise de variância one-way e teste de Tukey, com nível de significância de 5%. A análise por MEV demonstrou aglomeração das NPs CHX-HMP, o diâmetro médio efetivo aferido por DLS foi de 169,39 nm e o potencial zeta foi de -10,18 mV. As NPs foram mensuradas por AFM, apresentando: 22,99 a 52,75 nm. Os elementos químicos: C, N, O, Na, P, Cl, identificados por EDS, comprovam a interação entre o digluconato de CHX e HMP. A ação antimicrobiana das NPs confirmou-se preliminarmente no teste de difusão em ágar e o DCT demonstrou o aumento da ação antimicrobiana dos cimentos endodônticos após incorporação das NPs, principalmente no MTA Fillapex, eliminando totalmente as cepas após 30 dias. A citotoxicidade dos cimentos analisados não foi potencializada pelas NPs. Houve redução do escoamento após a incorporação das NPs, no entanto sem infringir a norma ISO 6876:2012. A incorporação de NPs não alterou a radiopacidade das amostras, mas o MTA Fillapex não atingiu a radiopacidade mínima preconizada. As amostras incorporadas apresentaram redução da solubilidade após 24h de imersão, no entanto o MTA Fillapex em todas as amostras excedeu os valores preconizados pela ISO 6876:2012. Quanto ao pH, todas as amostras apresentaram decréscimo do valor com a progressão do tempo de imersão. O tempo de presa do AH Plus aumentou após a incorporação das NPs e o MTA Fillapex não atingiu a presa em nenhuma das condições testadas. Com os resultados obtidos conclui-se que a incorporação das NPs pode beneficiar o desempenho antimicrobiano dos cimentos endodônticos.(AU)

This study evaluated the influence of the incorporation of chlorhexidine hexametaphosphate NPs in various properties of the following endodontic sealers: AH Plus, MTA Fillapex and Pulp Canal Sealer (PCS). The NPs were synthesized using a suspension containing 5 mM sodium hexametaphosphate (HMP) and 4 mM 20% chlorhexidine digluconate (CHX), and characterized by scanning electron microscopy (SEM), dynamic light scattering (DLS), zeta potential, atomic force microscopy (AFM), energy-dispersive X-ray spectroscopy (EDS). Endodontic sealers were incorporated by weight of 2% and 5% of NPs. The antimicrobial activity of the samples was evaluated by agar diffusion test and direct contact (DCT) against E. faecalis. DCT was conducted in 3 storage times: fresh sealers (T0), after 7 days (T7) and after 30 days (T30) storage, and two contact times with E. faecalis suspension for 10 and 60 minutes. The cytotoxicity of the samples was evaluated according to ISO 10993-12 standards, through extracts prepared in Eagle modified by Dulbecco culture medium. The interactions of MRC-5 fibroblasts cell culture with the extracts serial dilutions (1: 1 to 1: 8) were analyzed by tetrazolium mitochondrial metabolism quantification assay (MTT). Samples flow, radiopacity, solubility and setting time were evaluated according to ISO 6876: 2012. Solubility was evaluated after 24 hours and 7 days of sample immersion and the pH measured after: 3h, 24h, 48h, 72h and 7 days of storage. The results were submitted to statistical analysis by one-way analysis of variance test and Tukey test, with a significance level of 5%. SEM analysis showed a tendency for CHX-HMP NPs to cluster, the effective mean diameter measured by DLS was 169,39 nm and the zeta potential: -10.18 mV. The NPs were individually measured by AFM, showing: 22.99 to 52.75 nm. The chemical elements: C, N, O, Na, P, Cl, identified by EDS, prove the interaction between CHX digluconate and HMP. The antimicrobial action of NPs was preliminarily confirmed in the agar diffusion test and the DCT demonstrated an increase in the antimicrobial action of endodontic sealers after incorporation of NPs, mainly in the MTA Fillapex, totally eliminating the strains after 30 days. There was reduction of flow after NPs incorporation, however without violating the ISO 6876: 2012 standard. The incorporation of NPs did not change the radiopacity of the samples, but MTA Fillapex did not reach the minimum radiopacity recommended. The incorporated samples showed reduced solubility after 24 hours of immersion, however the MTA Fillapex in all samples exceeded the values recommended by ISO 6876:2012.. Regarding the pH, all samples showed a decrease in the value as the immersion time progressed. AH Plus setting time increased after incorporation of NPs and MTA Fillapex did not reached setting under none of the conditions tested. With the obtained results it can be concluded that the incorporation of NPs can benefit the antimicrobial performance of endodontic sealers.(AU)

Preparation and characterization of naftifine-loaded poly(vinyl alcohol)/sodium alginate electrospun nanofibers

In this study, naftifine (a topical antifungal drug) loaded poly(vinyl) alcohol (PVA)/sodium alginate (SA) nanofibrous mats were prepared using the single-needle electrospinning technique. The produced nanofibers were crosslinked with glutaraldehyde (GTA) vapor. The morphology and diameter of the electrospun nanofibers were studied by scanning electron microscopy (SEM). SEM images showed the smoothness of the nanofibers and indicated that the fiber diameter increased with crosslinking and drug loading. Atomic force microscopy (AFM) images confirmed the uniform production of the scaffolds, and elemental mapping via energy dispersive X-ray spectroscopy (EDS) showed the uniform distribution of the drug within the nanofibers. An attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy study demonstrated that naftifine has sufficient secondary interactions with the polymer blend. The crosslinking treatment decreased the burst drug release effectively and the release mechanism followed Korsmeyer-Peppas Super Case-II transport. Overall, these findings suggest the potential use of naftifine-loaded PVA/SA nanofibers as a topical antifungal drug delivery system.

Effect of hydrofluoric acid-based etchant at an elevated temperature on the bond strength and surface topography of Y-TZP ceramics

OBJECTIVES: This study investigated the effects of a hydrofluoric acid (HA; solution of hydrogen fluoride [HF] in water)-based smart etching (SE) solution at an elevated temperature on yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) ceramics in terms of bond strength and morphological changes.MATERIALS AND METHODS: Eighty sintered Y-TZP specimens were prepared for shear bond strength (SBS) testing. The bonding surface of the Y-TZP specimens was treated with 37% phosphoric acid etching at 20°C–25°C, 4% HA etching at 20°C–25°C, or HA-based SE at 70°C–80°C. In all groups, zirconia primers were applied to the bonding surface of Y-TZP. For each group, 2 types of resin cement (with or without methacryloyloxydecyl dihydrogen phosphate [MDP]) were used. SBS testing was performed. Topographic changes of the etched Y-TZP surface were analyzed using scanning electron microscopy and atomic force microscopy. The results were analyzed and compared using 2-way analysis of variance.RESULTS: Regardless of the type of resin cement, the highest bond strength was measured in the SE group, with significant differences compared to the other groups (p < 0.05). In all groups, MDP-containing resin cement yielded significantly higher bond strength values than MDP-free resin cement (p < 0.05). It was also shown that the Y-TZP surface was etched by the SE solution, causing a large change in the surface topography.CONCLUSIONS: Bond strength significantly improved when a heated HA-based SE solution was applied to the Y-TZP surface, and the etched Y-TZP surface was more irregular and had higher surface roughness.

Increased elastic modulus of the synovial membrane in a rat ACLT model of osteoarthritis revealed by atomic force microscopy

This study aimed to explore changes in nanoscale elastic modulus of the synovium using atomic force microscopy (AFM) in addition to investigate changes in synovial histomorphology and secretory function in osteoarthritis (OA) in a rat anterior cruciate ligament transection (ACLT) model. Sprague-Dawley rats were randomly assigned to sham control and ACLT OA groups. All right knee joints were harvested at 4, 8, or 12 weeks (W) after surgery for histological assessment of cartilage damage and synovitis in both the anterior and posterior capsules. AFM imaging and nanoscale biomechanical testing were conducted to measure the elastic modulus of the synovial collagen fibrils. Immunohistochemistry was used to visualize the expression of interleukin-1β (IL-1β), tumor necrosis factor-α (TNF-α), and matrix metalloproteinase-3 (MMP-3) in the synovium. The OA groups exhibited progressive development of disease in the cartilage and synovium. Histopathological scores of the synovium in the OA groups increased gradually. Significant differences were observed between all OA groups except for the posterior 4W group. The synovial fibril arrangement in all OA groups was significantly disordered. The synovial fibrils in all ACLT OA groups at each time point were stiffer than those in the sham controls. OA rats displayed a significantly higher expression of IL-1β and MMP3 in the anterior capsule. In summary, synovial stiffening was closely associated with joint degeneration and might be a factor contributing to synovitis and increased production of proinflammatory mediators. Our data provided insights into the role of synovitis, particularly stiffening of the synovium, in OA pathogenesis.

Effect of diode laser irradiation on the bond strength of polymerized non-simplified adhesive systems after 12 months of water storage

Abstract Objectives: The aim of this in vitro study was to evaluate the bonding strength of non-simplified dentin bonding systems (DBS) to dentin irradiated with a diode laser (970 nm) immediately and after 12 months of water storage following either primer or bond application. Material and methods: The experimental design included three different factors: DBS type [AdperTM Scotchbond Multipurpose (MP) and Clearfil™ SE Bond (CSE)], irradiation [without irradiation - control (C), irradiation after primer application (AP), and irradiation after bond application (AB)], and time [initial (I) and after 12 months of water storage (12 m)]. Sixty sound human third molars (n = 10) were obtained, and their flat occlusal dentin areas were prepared and standardized. Laser irradiation was performed in the contact mode perpendicular to the dental surface over an automatically selected scanning area at a pulse energy of 0.8 W, frequency of 10 Hz, and energy density of 66.67 J/cm2. After 7 days of treatment, the specimens were cut, and half of them were subjected to microtensile testing (500 N/0.05 mm/min), whereas the remaining sticks were examined after 12 months of water storage. The obtained data were analyzed by three-way analysis of variance (ANOVA) followed by a Tukey test (p<0.05). The observed fracture modes were investigated using a portable digital microscope with a magnification of 40x. Results: Among the utilized DBS, MP generally exhibited higher bond strengths, but did not always differ from CSE under similar conditions. The irradiation factor was statistically significant only for the MP/AB groups. After 12 months of storage, all groups demonstrated a significant reduction in the bond strength, whereas the results of fracture analysis showed a predominance of the adhesive type. Conclusions: The laser treatment of non-simplified DBS was not able to stabilize their bonding characteristics after 12 months.

Effect of grape seed extract-containing phosphoric acid formulations on bonding to enamel and dentin

Abstract The aim was to evaluate the effect of 2% grape seed extract (GSE) containing phosphoric acid (PhA) on the bond strength to enamel and dentin. The control group was 37% PhA. The following three PhA formulations with 2% GSE and 20% ethanol were obtained: GSE5 = 5% PhA; GSE10 = 10% PhA; and GSE20 = 20% PhA. The enamel and dentin surfaces of molars were etched with the acid solutions, followed by Scotchbond Multi-Purpose adhesive and composite resin application. The tensile bond strength (TBS) test evaluated the bond to enamel after 24 h, and the microtensile bond strength (μTBS) test evaluated the bond to dentin after 24 h and 12-month water storage. Etched enamel and dentin were observed by scanning electron microscopy (SEM) and atomic force microscopy (AFM), respectively. The TBS data were submitted to one-way ANOVA, while µTBS data were submitted to two-way ANOVA and Tukey's test (α = 0.05). The TBS (MPa) to enamel did not significantly differ among the control (48.1 ± 15.7), GSE5 (46.1 ± 9.6), GSE10 (49.8 ± 13.6) and GSE20 (44.1 ± 11.9) groups (p = 0.537). The µTBS (MPa) to dentin of the control (28.4 ± 14.4) and GSE20 (24.1 ± 8.1) groups were significantly higher than those of the GSE5 (16.8 ± 7.4) and GSE10 (17.5 ± 6.6) groups at 24 h (p < 0.006). After 12-month storage, only GSE5 (21.0 ± 7.8) and GSE10 (17.6 ± 8.0) did not show significantly decreased μTBS (p > 0.145). SEM micrographs showed a shallower enamel etching pattern for GSE5. AFM images showed the formation of collagenous globular structures for GSE5 and GSE10. The different acid solutions did not influence the TBS to enamel, and the µTBS to dentin was stable over time when dentin was etched with GSE5 and GSE10.

Additive manufacturing of titanium alloy could modify the pathogenic microbial profile: an in vitro study

Abstract Additive manufacturing (AM) is an emerging process for biomaterials and medical devices. Direct Laser Metal Sintering (DLMS) is an AM technique used to fabricate Ti-6Al-4V implant materials with enhanced surface-related properties compared with wrought samples; thus, this technique could influence microbial adsorption and colonization. Therefore, this in vitro study was conducted to evaluate the impact of different implant production processes on microbial adhesion of periodontal pathogens. Titanium discs produced using two different processes—conventional and AM—were divided into three groups: conventional titanium discs with machined surface (G1), AM titanium discs with chemical treatment (G2) and AM titanium discs without chemical treatment (G3). Subgingival biofilm composed of 32 species was formed on the titanium discs, and positioned vertically in 96-well plates, for 7 days. The proportions of microbial complexes and the microbial profiles were analyzed using a DNA-DNA hybridization technique, and data were evaluated using Kruskal-Wallis and Dunnett tests (p < 0.05). Lower proportions of the red complex species were observed in the biofilm formed in G2 compared with that in G1 (p < 0.05). Moreover, the proportions of the microbial complexes were similar between G2 and G3 (p > 0.05). Compared with G1, G2 showed reduced levels of Porphyromonas gingvalis , Actinomyces gerencseriae, and Streptococcus intermedius , and increased levels of Parvimonas micra , Actinomyces odontolyticus, and Eikenella corrodens (p < 0.05). The microbial profile of G3 did not differ from G1 and G2 (p > 0.05). The results of this in vitro study showed that titanium discs produced via AM could alter the microbial profile of the biofilm formed around them. Further clinical studies should be conducted to confirm these findings.

Surface morphologic evaluation of orthodontic bonding systems under conditions of cariogenic challenge

Abstract: Orthodontic bonding systems are submitted to demineralization and remineralization dynamics that might compromise their surface smoothness, and favor biofilm aggregation and caries development. The aim of the present study was to evaluate the effects of a cariogenic challenge model (in vitro pH-cycling model) on the surface roughness and topography of 3 bonding materials: Transbond™ XT (XT), Transbond™ Plus Color Change (PLUS) and Fuji Ortho™ LC (FUJI), by means of Atomic Force Microscopy (AFM). Six specimens with standardized dimensions and surface smoothness were fabricated per group, and the materials were manipulated in accordance with the manufacturers' instructions. No polishing was necessary. AFM tests were performed before and after pH-cycling, taking 3 readouts per specimen. The roughness results (Ra) were obtained at nanometric levels (nm) and surface records were acquired in two- and three-dimensional images of height and lock-in phase of the material components. The surfaces of all groups analyzed in the study were morphologically altered, presenting images suggestive of matrix degradation and loss of matrix-load integrity. FUJI presented the greatest increase in surface roughness, followed by XT and PLUS, respectively (p≤0.001). Nevertheless, the roughness values found did not present sufficient degradation to harbor bacteria. The surface roughness of all tested materials was increased by pH-cycling. The use of materials capable of resisting degradation in the oral environment is recommended, in order to conserve their integrity and of the surrounding tissues.

Caracterização interna de materiais restauradores indiretos com diferentes condicionamentos de superfície / Internal characterization of indirect restorative materials with different surface etching protocols

Objetivo: O objetivo do estudo foi avaliar o efeito da aplicação de ácido fluorídrico com diferentes tempos e concentrações na superfície de materiais restauradores indiretos obtidos a partir de blocos utilizados na tecnologia CAD-CAM. Materiais e Métodos: Amostras dos materiais restauradores indiretos medindo 4x4x0,8mm foram obtidos a partir de blocos CAD para cada material estudado: resina nanocerâmica Lava Ultimate (3M Espe), monossilicato de lítio reforçado por zircônia Celtra Duo (Dentsply) e cerâmica híbrida Vita Enamic (Vita). Os materiais foram submetidos à aplicação de ácido fluorídrico com concentração de 5% ou 10%, sendo o mesmo aplicado pelos tempos de 20, 40, 60 ou 90 segundos. Um grupo controle para cada material foi avaliado, sem nenhum tratamento de superfície, contabilizando nove grupos de cada material (n=10). As amostras foram avaliadas em relação à rugosidade de superfície (Ra e Rz), avaliadas em microscopia óptica confocal; ângulo de contato (θ), energia de superfície (s) e energia livre total de interação (∆G) avaliados em goniômetro, e resistência de união ao cimento resinoso avaliada através do teste de microcisalhamento. Imagens das amostras foram obtidas em microscopia eletrônica de varredura (MEV), microscopia óptica confocal e microscopia de força atômica. Os dados de rugosidade de superfície, ângulo de contato, energia de superfície, energia livre total de interação e resistência de união foram submetidos à ANOVA dois fatores e teste de Tukey (p<0,05). Resultados: Os resultados mostraram que, de maneira geral, o monosilicato de lítio reforçado por zircônia Celtra Duo apresentou melhores resultados quando submetido ao condicionamento com ácido fluorídrico 10% por 40 ou 60 segundos de aplicação. A resina nanocerâmica Lava Ultimate apresentou melhor performance quando condicionada com ácido fluorídrico 10% por 20 ou 40 segundos, enquanto que a cerâmica híbrida Vita Enamic apresentou melhores resultados quando condicionada com ácido fluorídrico 5% por 90 segundos. Conclusão: Cada material interagiu de maneira diferente ao condicionamento com ácido fluorídrico, sendo que o conhecimento do adequado protocolo para cada material é essencial para garantir melhorias nos processos de adesão e durabilidade das restaurações indiretas. Celtra Duo apresentou de maneira geral propriedades mecânicas superiores aos demais. Relevância clínica: Recomenda-se protocolos específicos de tratamento de superfície com ácido fluorídrico de acordo com a composição de cada material restaurador indireto(AU)

Purpose: The aim of this study was to evaluate the effect of different times and concentration of hydrofluoric acid etching on the surface of indirect restorative materials obtained from blocks used in CAD-CAM technology. Methods and Materials: Samples of indirect restorative materials measuring 4x4x0.8mm were obtained for each restorative material studied: Lava Ultimate nanoceramic resin (3M Espe), Celtra Duo zirconia-reinforced lithium silicate ceramic (Dentsply) and Vita Enamic polymer-infiltrated ceramic-network material (Vita). The materials were submitted to etching with 5% or 10% hydrofluoric acid for 20, 40, 60 or 90 seconds. A control group for each material was evaluated without any surface treatment, totaling nine experimental groups for each material (n = 10). The samples were evaluated in relation to surface roughness (Ra and Rz), evaluated by confocal optical microscopy; contact angle (θ), surface energy (s) and total free interaction energy (∆G) evaluated by goniometer; and microshear bond strength to resin cement. Sample images were obtained by scanning electron microscopy (SEM), confocal optical microscopy and atomic force microscopy. Data of surface roughness, contact angle, surface energy, total free interaction energy and bond strength were submitted to two-way ANOVA and Tukey test (p<0.05). Results: The results showed that, in general, the Celtra Duo zirconia-reinforced lithium silicate ceramic showed better results when subjected to etching with 10% hydrofluoric acid for 40 or 60 seconds. Lava Ultimate nanoceramic resin showed better performance when etched with 10% hydrofluoric acid for 20 or 40 seconds, while Vita Enamic polymer-infiltrated ceramic-network showed better results when etched with 5% hydrofluoric acid for 90 seconds. Conclusion: Each material showed different characteristics after etching with hydrofluoric acid, and the knowledge of the proper protocol for each material is essential to ensure improvements in the adhesion process and durability of indirect restorations. Celtra Duo presents general ways of mechanical properties superior to the others. Clinical relevance: Specific surface treatment protocols with hydrofluoric acid are recommended based on the different compositions of indirect restorative materials(AU)

Mechanical and Mechanosensing Properties of Tumor Affected Bone Cells Were Inhibited via PI3K/Akt Pathway

BACKGROUND: Osteolytic metastasis is a common destructive form of metastasis, in which there is an increased bone resorption but impaired bone formation. It is hypothesized that the changed mechanical properties of tumor affected bone cells could inhibit its mechanosensing, thus contributing to differences in bone remodeling. METHODS: Here, atomic force microscopy indentation on primary bone cells exposed to 50% conditioned medium from Walker 256 (W) carcinoma cell line or its adaptive tumor (T) cells was carried out. Nitric oxide levels of bone cells were monitored in response to low-magnitude, high-frequency (LMHF) vibrations. RESULTS: A stronger sustained inhibitive effect on bone cell viability and differentiation by T cells as compared to that of its cell line was demonstrated. This could be attributed to the higher levels of transforming growth factor-β1 (TGF-β1) in the T-conditioned medium as compared to W-conditioned medium. Bone cell elastic moduli in W and T-groups were found to decrease significantly by 61.0% and 69.6%, respectively compared to control and corresponded to filamentous actin changes. Nitric oxide responses were significantly inhibited in T-conditioned group but not in W-conditioned group. CONCLUSIONS: It implied that a change in cell mechanical properties is not sufficient as an indicator of change in mechanosensing ability. Moreover, inhibition of phosphoinositide 3-kinase/Akt downstream signaling pathway of TGF-β1 alleviated the inhibition effects on mechanosensing in T-conditioned cells, further suggesting that growth factors such as TGF-β could be good therapeutic targets for osteoblast treatment.

Effects of different finishing/polishing protocols and systems for monolithic zirconia on surface topography, phase transformation, and biofilm formation

PURPOSE: The purpose of this study was to evaluate the effects of various protocols and systems for finishing and polishing monolithic zirconia on surface topography, phase transformation, and bacterial adhesion. MATERIALS AND METHODS: Three hundred monolithic zirconia specimens were fabricated and then treated with three finishing and polishing systems (Jota [JO], Meisinger [ME], and Edenta [ED]) using four surface treatment protocols: coarse finishing alone (C); coarse finishing and medium polishing (CM); coarse finishing and fine polishing (CF); and coarse finishing, medium polishing, and fine polishing (CMF). Surface roughness, crystal phase transformation, and bacterial adhesion were evaluated using atomic force microscopy, X-ray diffraction, and streptococcal biofilm formation assay, respectively. One-way and two-way analysis of variance with Tukey post hoc tests were used to analyze the results (α=.05). RESULTS: In this study, the surface treatment protocols and systems had significant effects on the resulting roughness. The CMF protocol produced the lowest roughness values, followed by CM and CF. Use of the JO system produced the lowest roughness values and the smallest biofilm mass, while the ME system produced the smallest partial transformation ratio. The ED group exhibited the highest roughness values, biofilm mass, and partial transformation ratio. CONCLUSION: Stepwise surface treatment of monolithic zirconia, combined with careful polishing system selection, is essential to obtaining optimal microstructural and biological surface results.

Surface analysis of metal clips of ceramic self-ligating brackets / 대한치과교정학회지

OBJECTIVE: The aim of this study was to analyze the surface composition, roughness, and relative friction of metal clips from various ceramic self-ligating brackets. METHODS: Six kinds of brackets were examined. The control group (mC) consisted of interactive metal self-ligating brackets while the experimental group (CC, EC, MA, QK, and WA) consisted of interactive ceramic self-ligating brackets. Atomic force microscopy-lateral force microscopy and scanning electron microscopy-energy-dispersive X-ray spectroscopy were used to analyze the surface of each bracket clip. RESULTS: All the clips in the experimental groups were coated with rhodium except for the QK clip. The results showed that the QK clip had the lowest average roughness on the outer surface, followed by the MA, EC, WA, and CC clips. However, the CC clip had the lowest average roughness on the inner surface, followed by the QK, WA, MA, and EC clips. The QK clip also had the lowest relative friction on the outer surface, followed by the MA, EC, CC, and WA clips. Likewise, the CC clip had the lowest relative friction on the inner surface, followed by the QK, WA, MA, and EC clips. CONCLUSIONS: The surface roughness and relative friction of the rhodium-coated clips were generally higher than those of the uncoated clips.

Polishing of ground y-tzp ceramic is mandatory for improving the mechanical behavior

Abstract It evaluated the effect of aging by Low Temperature Degradation (LTD), executed after post- processing surface treatments (polishing, heat treatment and glazing), on the surface characteristics (micromorphology and roughness) and on the structural stability (phase transformation and mechanical behavior-flexural strength and structural reliability) of a ground yttrium-stabilized tetragonal zirconia polycrystal (Y-TZP) ceramic. Discs of Y-TZP (VITA In-Ceram YZ) were manufactured (ISO:6872-2015; 15 mm in diameter and 1.2 ± 0.2 mm in thickness) and randomly assigned into 10 groups according two factors: "aging" in 2 levels (with or without) and "surface treatment" in 5 levels (Ctrl: as-sintered; Gr: grinding with coarse diamond bur; Gr + HT: grinding plus heat treatment; Gr + Pol: grinding plus polishing; Gr + Gl: grinding plus glazing). Roughness (n=30), biaxial flexural test (n=30), phase transformation (n=2), and surface topography (n=2) analyses were performed. Aging led to an intense increase in monoclinic (m) phase content for all the tested conditions, being the as-sintered samples (Ctrl= 65.6%) more susceptible to the t-m phase transformation. Despite of increasing the m-phase content, aging was not detrimental for characteristic strength (except to the grinding condition). There was no significant reduction in the Weibull modulus after surface treatments. Additionally, heat treatment and glazing after grinding led to a decrease in characteristic strength, while polishing presented the highest characteristic strength values. Thus, polishing is mandatory after grinding the Y-TZP ceramic, while performing glazing or heat-treatment alone after grinding lead to the worst mechanical performance.

Resumo Este estudo avaliou o efeito do envelhecimento através da degradação a baixas temperaturas (low temperaturare degradation - LTD) após a realização de tratamentos de superfície pós- sinterização (polimento, tratamento térmico e glaze) nas características superficiais (micromorfologia e rugosidade), e na estabilidade estrutural (transformação de fase e comportamento mecânico - resistência flexural e confiabilidade estrutural) de uma cerâmica de zircônia tetragonal policristalina estabilizada por ítria (Y-TZP) desgastada. Discos de cerâmica Y-TZP (VITA In-Ceram YZ) foram confeccionados (ISO:6872-2015; 15mm de diâmetro e 1,2 ± 0,2mm de espessura) e randomicamente divididos em 10 grupos de acordo com dois fatores: "envelhecimento" (com e sem) e "tratamento de superfície" (Ctrl - sem tratamento; Gr - desgaste com ponta diamantada grossa; Gr + HT - desgaste mais tratamento térmico; Gr + Pol - desgaste mais polimento; Gr + Gl - desgaste mais glazeamento). Foram realizadas as análises de rugosidade (n=30), flexão biaxial (n=30), transformação de fase (n=2) e topografia de superfície (n=2). O envelhecimento levou a um aumento intenso no conteúdo de fase monoclínica (m) em todas as condições testadas, sendo observada uma maior susceptibilidade de transformação de fase t-m nas amostras do grupo controle (Ctrl= 65.6%). Apesar de provocar elevada transformação de fase, o envelhecimento não apresentou efeitos negativos nos desfechos avaliados. Não houve redução significativa do módulo de Weibull após os tratamentos. Além disso, o tratamento térmico e o glaze após desgaste levaram a uma redução da resistência característica, enquanto que o grupo polimento apresentou o mais alto valor de resistência característica. O glaze e o tratamento térmico geraram o pior desempenho mecânico, portanto a realização do polimento após desgaste de uma cerâmica Y-TZP é obrigatória.

Adhesion to a lithium disilicate glass ceramic etched with hydrofluoric acid at distinct concentrations

Abstract This study evaluated the effect of different hydrofluoric acid (HF) concentrations on the bond strength between a lithium disilicate-based glass ceramic and a resin cement. Eighty ceramic-blocks (12×7×2 mm) of IPS e.Max CAD (Ivoclar Vivadent) were produced and randomly assigned to 8 groups, considering 2 study factors: HF concentration in 4 levels, i.e., 1% (HF1), 3% (HF3), 5% (HF5), and 10% (HF10), and storage in 2 levels, i.e., baseline (tests were performed 24 h after cementation), and aged (storage for 150 days + 12,000 thermal-cycles at 5°C and 55°C). Acid etching (20 s) was performed, followed by washing, drying, and silanization. Four resin cement cylinders (ϕ= 0.96 mm) were built-up from starch matrices on each ceramic sample (n= 40). Additional ceramic samples were etched and analyzed for contact angle, micro-morphology, and roughness. In baseline condition (without aging), the HF3, HF5, and HF10 groups showed similar bond strength values (13.9 - 15.9 MPa), and HF1 (11.2 MPa) presented lower values than HF5, being that statistically different (p= 0.012). After aging, all the mean bond strengths statistically decreased, being that HF3, HF5, and HF10 (7.8 - 11 MPa) were similar and higher than HF1 (1.8 MPa) (p= 0.0001). For contact angle, HF3, HF5, and HF10 presented similar values (7.8 - 10.4°), lower than HF1 and CTRL groups. HF5 and HF10 presented rougher surfaces than other conditions. For better bond strength results, the tested ceramic may be etched by HF acid in concentrations of 3%, 5%, and 10%.

Resumo Este estudo avaliou o efeito de diferentes concentrações de ácido fluorídrico (HF) na resistência de união entre uma cerâmica vítrea à base de dissilicato de lítio e um cimento resinoso. Oitenta blocos cerâmicos (12×7×2 mm) de IPS e.Max CAD (Ivoclar Vivadent) foram produzidos e distribuídos aleatoriamente em 8 grupos, considerando 2 fatores de estudo: concentração de HF em 4 níveis, isto é, 1% (HF1), 3% (HF3), 5% (HF5), e 10% (HF10), e armazenamento em 2 níveis, isto é, condição inicial (testes foram realizados 24 h após a cimentação), e envelhecidos (150 dias de armazenamento + 12.000 ciclos térmicos a 5°C e 55°C). Condicionamento ácido (20 s) foi realizado, seguido por lavagem, secagem e silanização. Quatro cilindros de cimento resinoso (ϕ= 0.96 mm) foram construídos a partir de matrizes de amido em cada amostra cerâmica (n= 40). Amostras cerâmicas adicionais foram condicionadas e analisadas quanto ao ângulo de contato, micro-morfologia e rugosidade. Na condição inicial (sem envelhecimento), os grupos HF3, HF5, e HF10 mostraram valores de resistência de união similares (13.9 - 15.9 MPa), e HF1 apresentou valores menores que HF5, sendo estatisticamente diferente (p= 0.012). Após o envelhecimento, todas as médias de resistência de união diminuíram estatisticamente, sendo que HF3, HF5 e HF10 foram similares e maiores que HF1 (p= 0.0001). Para o ângulo de contato, HF3, HF5 e HF10 apresentaram valores similares (7.8 - 10.4°), menores que os grupos HF1 e CTRL. HF5 e HF10 apresentaram superfícies mais rugosas que as outras condições. Para melhores resultados de resistência de união, a cerâmica testada pode ser condicionada com ácido fluorídrico nas concentrações de 3%, 5% e 10%.

Physicomechanical characterization and biological evaluation of bulk-fill composite resin

Abstract The aim of this study was to evaluate the cytotoxic effect, degree of conversion (% DC), Vickers hardness (VH), and surface morphology of composite resins. Eleven resins, nine bulk-fill resins, and two conventional resins were evaluated. Each material was sampled to evaluate DC (using FTIR), VH, cytotoxicity (using MTT and Neutral Red - NR test), surface morphology (using SEM and AFM), and organic filler (using EDS). All statistical tests were performed with SPSS and the level of significance was set at 0.05. MTT revealed that the materials presented low or no cytotoxic potential in relation to the control. Opus was the resin with the lowest cell viability at a 1:2 concentration at 72 h (32%) and at 7 days (43%), but that significantly increased when the NR test was applied at a 1:2 concentration after 7 days. Thickness and surface subjected to polymerization had no influence on DC, and differences were observed only between the materials. In the microhardness test, statistical differences were observed between the evaluated thicknesses. The bulk-fill resins analyzed in this study exhibited low and/or no cytotoxicity to L929 cells, except for Opus, which showed moderate cytotoxicity according to the MTT assay. When the NR test was used, results were not satisfactory for all composites, indicating the need for different methodologies to evaluate the properties of these materials. The assessed resins demonstrated acceptable physicomechanical properties.

Impacto de um método de polimento adicional em propriedades físicas, micromorfológicas e microtopográficas de compósitos convencionais e Bulk Fill / Impact of an additional polishing method on physical, micromorphological and microtopographical properties of conventional and Bulk Fill composites

O objetivo deste trabalho foi avaliar a rugosidade superficial, a molhabilidade, a disposição em profundidade das partículas de carga, o mapeamento de elementos químicos, a microtopografia em 3D e a micromorfologia de compósitos convencionais e bulk fill após polimento adicional. Éspécimes foram preparados de cada compósito testado, sendo quatro do tipo bulk fill (Filtek Bulk, Fill Tetric N-Ceram Bulk Fill, Opus Bulk Fill e X-tra Fil) e quatro convencionais (Filtek Z250 XT, Grandioso, Tetric NCeram, Vittra APS), de acordo com três técnicas de acabamento/polimento/polimento adicional (n = 10): sem acabamento e polimento, acabamento e polimento com borrachas abrasivas (Astropol), acabamento e polimento com Astropol mais polimento adicional com escova de carbeto de silício. A rugosidade superficial (Ra) e o ângulo de contato foram medidos usando-se um perfilômetro e goniômetro adaptado, respectivamente. A microtopografia 3D foi avaliada utilizando microscopia de força atômica (MFA), enquanto a micromorfologia e a disposição em profundidade das partículas de carga, através da microscopia eletrônica de varredura (MEV). O mapeamento de elementos químicos foi avaliado por meio de Espectroscopia por energia dispersiva de raio-X (EDS). A rugosidade e o ângulo de contato foram analisados pelo ANOVA-dois fatores e teste de Tukey (p <0,05); os demais dados foram analisados descritivamente. A disposição das partículas de carga em profundidade de todas as resinas envolvidas neste estudo apresentou uma camada superficial rica em matriz orgânica e uma camada subsuperficial rica em partículas de dimensões mais diminutas. O polimento adicional: diminuiu a rugosidade superficial das resinas Filtek Bulk Fill, Vittra APS, Tetric N-ceram Bulk Fill e X-tra fil; aumentou o valor do ângulo de contato da X-tra Fil e diminuiu da Filtek Z250 XT. Nas análises para microtopografia em 3D e a micromorfologia, superfícies mais lisas e uniformes foram observadas em todas as resinas. Os elementos: carbono (C), cxigênio (O), silício (Si), zircônia (Zr) e alumínio (Al) foram presentes em todas as resinas compostas. O bário (Ba) foi ausente na Filtek Z250 XT, Filtek Bulk Fil e Vittra APS. O carbono foi predominante em todas as resinas. Após polimento adicional, houve um aumento na detecção de oxigênio para todas as resinas, exceto para Tetric N-Ceram e Xtra Fil e uma diminuição de carbono, exceto para a Tetric N-Ceram Bulk Fil. O silício diminuiu apenas nas resinas Z250 XT, Tetric N-Ceram e Tetric N-Ceram Bulk Fill. A zircônia diminuiu para a Tetric N-Ceram Bulk Fill e o alumínio para Z250 XT e Tetric N-Ceram Bulk Fill. O bário aumentou para Opus Bulk fill e X-tra Fil. O titânio foi ausente para todas as resinas. Portanto, o polimento adicional melhorou as propriedades de superfície das resinas estudadas (AU).

The objective of this study was to evaluate the surface roughness, wettability, the depth distribution of the charge particles, the mapping of chemical elements, the 3D microtopography and the micromorphology of the composites of the conventional and bulk fill after additional polishing. The specimens were prepared from each of the composites tested, four of them being bulk fillers (Filtek Bulk Fill Tetric N-Ceram Bulk Fill Opus Bulk Fill X-tra Fil) and four conventional ones (Filtek Z250 XT, Grandioso, Tetric N-Ceram, Vittra APS ), according to three additional finishing / polishing / polishing techniques (n = 10): without finishing and polishing, finishing and polishing with abrasive rubbers (Astropol), finishing and polishing with Astropol plus additional polishing with silicon carbide brush. The surface roughness (Ra) and contact angles were measured using a profilometer and adapted goniometer, respectively. The 3D microtopography was evaluated using atomic force microscopy (AFM); while the micromorphology and the in-depth arrangement of the charge particles by scanning electron microscopy (SEM). The mapping of chemical elements was evaluated by means of X-ray Dispersive Energy Spectroscopy (EDS). The roughness and the contact angle were analyzed by ANOVA- two factors and Tukey test (p <0.05); the other data were analyzed descriptively. The arrangement of the in-depth charge particles of all the resins involved in this study had an organic matrix rich surface layer and a particulate rich subsurface layer of smaller dimensions. Addicional polishing: reduced surface roughness of Filtek Bulk Fill resins, Vittra APS, Tetric N-ceram Bulk Fill and X-trafil resins; increased the contact angle value of the X-tra Fil and decreased the Filtek Z250 XT. In the analyzes for 3D microtopography and micromorphology, smoother and more uniform surfaces were observed in all a resins. The elements: carbon (C), oxygen (O), silicon (Si), zirconia (Zr) and aluminum (Al) were present in all composite resins. Barium (Ba) was absent on Filtek Z250 XT, Filtek Bulk Fil and Vittra APS. Carbon was predominant in all resins. After additional polishing, there was an increase in oxygen detection for all resins except for Tetric N-Ceram and X-tra Fil and a decrease in carbon except for Tetric N-Ceram Bulk Fil. Silicon decreased only in the Z250 XT, Tetric N-Ceram and Tetric NCeram Bulk Fill resins. Zirconia decreased for Tetric N-Ceram Bulk Fill and aluminum for Z250 XT and Tetric N-Ceram Bulk Fill. Barium increased for Opus Bulk fill and X-tra Fil. Titanium was absent for all resins. Therefore, additional polishing improved the surface properties of the resins studied (AU).