Abstract This study evaluated the influence of non-thermal argon plasma applied to dentin on the shear strength of two adhesive systems. Ninety tooth fragments were embedded in epoxy resin and distributed into experimental groups (n=15): G1 and G4 - adhesive systems applied according to the manufacturers’ instructions; G2 and G5 - dentin treated with non-thermal argon plasma for 30 seconds before hybridization; G3 and G6 - dentin treated with non-thermal argon plasma for 30 seconds after hybridization. Cylinders were made with composite resin in the adhesive area, and the specimens were submitted to the shear strength test. Higher values were observed when applying the plasma treatment after hybridization (G1: 26.51 MPa, G2: 29.22 MPa, G3: 30.27 MPa, G4: 22.66 MPa, G5: 28.33 MPa, G6: 29.32 MPa). The treatment with non-thermal argon plasma significantly increased the shear strength values regardless of the application time.

Hydroxyapatite (HA) nanopowders are attracting interest for surface application to ceramic biomaterials. In this study, we developed innovative and new viable synthesis routes of calcium phosphate nanopowders from the natural calcium carbonate of chicken eggshells. Following the four routes, alternative co-precipitation, vacuum process, brushite, and calcination, we obtained the HA samples, which were then characterized by different methods. The X-ray diffraction /Rietveld method showed the HA phases, monetite and brushite crystallinity with greater symmetry, and nanoscale. Transmission electron microscopy showed the morphology of nanoparticles functionalized nanoparticles smaller than 100 nm in routes A, B and D, and Fourier-transform infrared spectrophotometry and Raman spectroscopy identified the classic chemical groups of calcium phosphates by four routes mainly groups (PO4)3- and (CO3-). Scanning electron microscopy analysis revealed a good surface topography to future cell biointeraction in A, B and D routes, and thermogravimetric analysis showed the mass loss profile inherent to each synthesis route with slot at 200 °C. Hence, the eggshell HA and brushite and the specific monetite nanoparticles with different morphology can be prepared from the four new possible and viable routes using different methods.

Resumo Introdução O tratamento de plasma é uma tecnologia eficaz que pode manter as propriedades internas dos materiais inalteradas após o tratamento, modificando apenas a superfície. Objetivo Avaliar o efeito do plasma de oxigênio na dentina previamente exposta ao NaOCl 6%. Material e método Foram utilizados 60 incisivos bovinos. A coroa foi removida, a raiz foi dividida e as faces planificadas, totalizando 120 segmentos referentes ao terço cervical. As amostras foram divididas em dois grupos: controle (imersa em NaOCl 6%, lavada com água destilada, seca, imersa em EDTA 17%, lavada e seca) e plasma de oxigênio (após tratamento descrito no grupo controle, plasma de oxigênio foi aplicado por 30 s). As amostras foram avaliadas qualitativamente em relação à topografia por microscopia eletrônica de varredura, utilizando-se microfotografias com ampliação de 1.000×. O goniômetro Ramé-hart foi utilizado para a mensuração do ângulo de contato entre as superfícies e as seguintes soluções foram utilizadas: água, etilenoglicol e di-iodometano. Em seguida, a energia de superfície, representada pelas componentes polar e dispersiva, foi calculada. Avaliou-se também o escoamento dos cimentos Pulp Canal Sealer EWT (PCS) e Real Sal SE (RS) na superfície dentinária. Os dados foram analisados estatisticamente utilizando os testes Kruskal-Wallis e Mann-Whitney U (p<0,05). Resultado O tratamento com plasma levou à formação de uma camada semelhante à smear layer na superfície dentinária. Este tratamento levou a um aumento da energia de superfície e da componente polar, favorecendo a hidrofilicidade da superfície. Entretanto, desfavoreceu o escoamento do cimento PCS e não influenciou no escoamento do cimento RS. Conclusão O plasma de oxigênio ocasionou mudanças topográficas na superfície dentinária, favorecendo a hidrofilicidade desta. Contudo, não favoreceu o escoamento dos cimentos endodônticos na dentina.

Abstract Introduction Plasma treatment is an effective technology since the internal properties of the material is kept unchanged after treatment, modifying only the surface. Objective To evaluate the effect of oxygen plasma on dentin previously exposed to 6% NaOCl. Material and method 60 bovine incisors were used. The crown was removed, the root splited and the faces planned amounting 120 segments related to the cervical third. The samples were divided into 2 groups, control (immersed in 6% NaOCl, washed with distilled water, dried, immersed in 17% EDTA, washed and dried) and oxygen plasma (after treatment described in the control group, oxygen plasma was applied for 30s). The samples were evaluated qualitatively in relation to topography by scanning electron microscopy using photomicrographs at 1000× of magnification. The Ramé-hart goniometer was used to measure the contact angle between the surfaces and the following solutions: water, ethyleneglycol, and diiodomethane. Then, surface energy, polar and dispersive components, was calculated. Additionally, it was evaluated the flow of Pulp Canal Sealer EWT (PCS) and Real Salt SE (RS) sealers on dentin surface. Data were statistically analyzed using Kruskal-Wallis e Mann-Whitney U (p<0.05). Result Plasma treatment caused topographical changes on dentin surface. This treatment led to an increase in surface energy and polar component, favoring the hydrophilicity of the surface. However, it disfavors the wettability of PCS and did not influence the RS wettability. Conclusion The oxygen plasma caused topographical changes on dentin surface, favoring its hydrophilicity. However, it did not favor the sealers wettability on dentin.

Resumo Estudos vêm demonstrando uma diminuição na resistência adesiva em dentina tratada com hipoclorito de sódio (NaOCl). O objetivo desse estudo foi avaliar o efeito do plasma de argônio não-térmico na resistência de união de um sistema adesivo autocondicionante à dentina exposta ao NaOCl. Trinta e duas superfícies dentinárias lisas de incisivos bovinos foram imersas em NaOCl a 2,5% por 30 min para simular o passo de irrigação durante o tratamento endodôntico. Os espécimes foram divididos em 4 grupos (n=8), de acordo com o tratamento de superfície: Controle (sem tratamento de plasma), AR15 (plasma de argônio por 15 s), AR30 (plasma de argônio por 30 s) e AR45 (plasma de argônio por 45 s). Para teste de resistência de união por microtração, cinco espécimes foram utilizadas por grupo. Em cada grupo, os espécimes foram hibridizados com um sistema adesivo autocondicionante (Clearfil SE Bond, Kuraray) e blocos de resina composta foram construídos. Após 48 h de armazenamento em água, os espécimes foram seccionados em palitos (5 por dente - 25 por grupo) e submetidos ao teste de resistência de união por microtração (μTBS) até a fratura, avaliando o padrão de fratura. Três amostras por grupo foram analisadas sob espectroscopia por FTIR para verificar as modificações químicas produzidas pelos tratamentos na dentina. Os dados de microtração foram avaliados estatisticamente utilizando os testes de ANOVA e Tamhane (p<0,05). AR30 apresentou o maior μTBS (20,86±9,0). AR15 (13,81±6,4) e AR45 (11,51±6,8) foram estatisticamente semelhantes ao controle (13,67±8,1). A espectroscopia por FTIR mostrou que o tratamento de plasma produziu modificações químicas na dentina. Como conclusão, o tratamento de plasma de argônio não-térmico por 30 s produziu alterações químicas na dentina e melhorou o μTBS do Clearfil SE Bond à dentina tratada com NaOCl.

Abstract Studies have been showing a decrease of bond strength in dentin treated with sodium hypochlorite (NaOCl). The aim of this study was to evaluate the effect of non-thermal argon plasma on the bond strength of a self-etch adhesive system to dentin exposed to NaOCl. Thirty-two flat dentin surfaces of bovine incisors were immersed in 2.5% NaOCl for 30 min to simulate the irrigation step during endodontic treatment. The specimens were divided into four groups (n=8), according to the surface treatment: Control (without plasma treatment), AR15 (argon plasma for 15 s), AR30 (argon plasma for 30 s) and AR45 (argon plasma for 45 s). For microtensile bond strength test, 5 specimens were used per group. In each group, the specimens were hybridized with a self-etch adhesive system (Clearfil SE Bond) and resin composite buildups were constructed. After 48 h of water storage, specimens were sectioned into sticks (5 per tooth, 25 per group) and subjected to microtensile bond strength test (μTBS) until failure, evaluating failure mode. Three specimens per group were analyzed under FTIR spectroscopy to verify the chemical modifications produced in dentin. μTBS data were analyzed using ANOVA and Tamhane tests (p<0.05). AR30 showed the highest μTBS (20.86±9.0). AR15 (13.81±6.4) and AR45 (11.51±6.8) were statistically similar to control (13.67±8.1). FTIR spectroscopy showed that argon plasma treatment produced chemical modifications in dentin. In conclusion, non-thermal argon plasma treatment for 30 s produced chemical changes in dentin and improved the μTBs of Clearfil SE Bond to NaOCl-treated dentin.

Resumo Introdução Os pinos de fibra de vidro são uma alternativa aos núcleos metálicos e apresentam vantagens, tais como: estética, módulo de elasticidade semelhante à dentina e cimentação imediata após o término do tratamento endodôntico. Ainda, apresentam a capacidade de aderir ao cimento resinoso e este, à dentina, por meio de técnicas adesivas. Objetivo Comparar a adesão de um cimento resinoso convencional e um autoadesivo a pinos de fibra de vidro, e os efeitos de diferentes tratamentos de superfície na resistência adesiva dos pinos. Material e método Trinta pinos foram divididos em três grupos: Controle: sem tratamento na superfície; Jateamento: jateamento com óxido de alumínio por 30 segundos, e Peróxido: imersão em peróxido de hidrogênio 24% por um minuto. Em seguida, corpos de prova foram obtidos a partir de cilindros de cimento resinoso contendo o pino de fibra posicionado no centro de seu longo eixo. Em cada grupo, cinco pinos foram associados ao adesivo Âmbar + cimento convencional AllCem Core e os outros cinco pinos, ao cimento autoadesivo RelyX U200. O conjunto pino/cimento foi segmentado e avaliado em relação à resistência de união (RU) por push-out. Os dados foram analisados estatisticamente pelos testes de ANOVA e Tukey (p<0,05). Resultado Os cimentos avaliados exibiram valores de RU semelhantes. Em relação aos tratamentos de superfície, os maiores valores de RU foram encontrados no grupo Jateamento. Conclusão O cimento convencional, AllCem Core, e o cimento autoadesivo, RelyX U200, mostraram valores de resistência de união semelhantes. Ainda, o jateamento com óxido de alumínio favoreceu a adesão dos pinos aos cimentos.

Abstract Introduction The fiberglass posts are an alternative to the metal cast, presenting some advantages, such as aesthetics, tensile modulus similar to dentin and can be placed in a single session, immediately after the endodontic treatment. It also has the ability to adhere to the resin cement and the last to dentin by means of bonding techniques. Objective To compare the adhesion of a conventional resin cement with a self-adhesive to fiberglass posts, and the effects of different surface treatments on adhesion of posts. Material and method Thirty fiber posts were divided into 3 groups: control: untreated surface; Blasting: blasting with aluminum oxide for 30 seconds and peroxide: immersion in 24% hydrogen peroxide for 1 minute. Then, the samples were obtained from resin cement cylinders containing the fiber post positioned in the center of its long axis. In each group 5 posts were associated with the adhesive Ambar+conventional cement Allcem Core and the other 5 posts with the self-adhesive cement RelyX U200. The post/cement sample was segment in discs and evaluated for bond strength (BS) by push-out test. Data were analyzed statistically by ANOVA and Tukey tests (p<0.05). Result The cements evaluated exhibited similar BS values. Regarding surface treatments, the highest BS values were found in blasting group. Conclusion Conventional cement, Allcem Core, and self-adhesive, RelyX U200, showed similar bond strength values. Also, blasting with aluminum oxide favored the adhesion of posts to cements.

Resumo O objetivo do presente estudo foi avaliar o efeito do plasma de argônio na superfície dentinária após o uso de NaOCl 6%. As coroas de 60 incisivos bovinos foram removidas, as raízes clivadas e os segmentos planificados. Cento e vinte segmentos referentes ao terço cervical foram utilizados. As amostras foram divididas em dois grupos (n=60): Grupo Controle: imersos em NaOCl 6%, lavados, secos, imersos em EDTA 17%, lavados e secos e Grupo Argônio: após o tratamento descrito no grupo controle, foi aplicado plasma de argônio não térmico por 30 s. Em cada grupo, 10 amostras foram avaliadas por microscopia eletrônica de varredura. Outras dez amostras foram analisadas por espectroscopia no infravermelho por transformada de Fourier (FTIR). Trinta amostras foram analisadas com um goniômetro para medir o ângulo de contato entre a superfície dentinária e as soluções e determinar a energia livre de superfície. As últimas dez amostras foram utilizadas para avaliar a molhabilidade do cimento AH Plus. Os dados foram analisados estatisticamente usando os testes de Kruskal Wallis e Mann-Whitney (p<0,05). Os resultados do estudo mostraram que o plasma de argônio não modificou a topografia de superfície. A análise por FTIR mostrou modificações químicas após o tratamento de plasma. O plasma de argônio aumentou a energia livre da superfície dentinária e a molhabilidade do cimento AH Plus. Conclusão, o tratamento com plasma de argônio modificou quimicamente a superfície dentinária. Este tratamento aumentou a energia livre de superfície e a molhabilidade de um cimento endodôntico à base de resina epóxi, favorecendo as características adesivas da superfície dentinária.

Abstract The aim of this study was to evaluate the effect of argon plasma on dentin surface after use of 6% NaOCl. Sixty bovine incisors had their crowns removed, the roots split, and the segments planed. One hundred twenty segments of the cervical third were used. The samples were divided in two groups (n=60): Control group: immersed in 6% NaOCl, washed, dried and then immersed in 17% EDTA, washed and dried and Argon group: after treatment described for the Control group, non-thermal argon plasma was applied for 30 s. Ten samples were evaluated by scanning electron microscopy in each group. Other ten samples were analyzed by Fourier transform infrared spectroscopy (FTIR). Thirty samples were analyzed with a goniometer to measure the contact angle between the dentin surfaces and solutions, to determine the surface free energy. The last ten samples were used to evaluate the wettability of AH Plus sealer. Data were statistically analyzed using Kruskal Wallis and Mann-Whitney tests (p<0.05). The results of this study showed that argon plasma did not modify the surface topography. FTIR analysis showed chemical modifications after plasma treatment. Argon plasma increased the surface free energy of dentin and AH Plus wettability. In conclusion, argon plasma treatment modified chemically the dentin surface. This treatment increased the surface free energy and wettability of an epoxy resin root canal sealer, favoring its bonding to dentin surfaces.

ABSTRACT Plasma technology has the potential to improve the adherence of fibers to polymeric matrices, and there are prospects for its application in dentistry to reinforce the dental particulate composite. Objectives This study aimed to investigate the effect of oxygen or argon plasma treatment on polyethylene fibers. Material and Methods Connect, Construct, InFibra, and InFibra treated with oxygen or argon plasma were topographically evaluated by scanning electron microscopy (SEM), and chemically by X-ray photoelectron spectroscopy (XPS). For bending analysis, one indirect composite (Signum) was reinforced with polyethylene fiber (Connect, Construct, or InFibra). The InFibra fiber was subjected to three different treatments: (1) single application of silane, (2) oxygen or argon plasma for 1 or 3 min, (3) oxygen or argon plasma and subsequent application of silane. The samples (25x2x2 mm), 6 unreinforced and 60 reinforced with fibers, were subjected to three-point loading tests to obtain their flexural strength and deflection. The results were statistically analyzed with ANOVA and the Bonferroni correction for multiple comparison tests. Results SEM analysis showed that oxygen and argon plasma treatments promote roughness on the polyethylene fiber surface. X-ray photoelectron spectroscopy (XPS) analysis shows that both plasmas were effective in incorporating oxygenated functional groups. Argon or oxygen plasma treatment affected the flexural strength and deflection of a fiber reinforced composite. The application of silane does not promote an increase in the flexural strength of the reinforced composites. Conclusions Oxygen and argon plasma treatments were effective in incorporating oxygenated functional groups and surface roughness. The highest strength values were obtained in the group reinforced with polyethylene fibers treated with oxygen plasma for 3 min.

Resumo O objetivo deste estudo foi avaliar o efeito do tratamento de plasma, utilizando os gases argônio e oxigênio, associado à posição da fibra, nas propriedades mecânicas de um compósito reforçado por fibra. Onze grupos foram avaliados, um grupo controle, sem reforço, e 10 grupos reforçados com Infibra, variando de acordo com o tratamento de plasma e a posição das fibra. As amostras foram preparadas utilizando uma matriz bipartida de aço inoxidável. O teste de flexão de três pontos foi realizado em uma máquina de ensaios EMIC. A resistência à flexão (FS) e deflexão (FD) foram calculados em relação à falha inicial (IF) e final (FF). Os dados foram avaliados estatisticamente pelos testes de Mann-Whitney e Kruskal-Wallis (p<0,05). Para IF, nas fibras posicionadas na base, os valores de FS e FD foram significativamente maiores do que quando as fibras foram afastadas da base em todos os grupos. O maior valor de FS foi obtido no grupo tratado com O 3 min (296,2 MPa) e o maior valor de FD foi obtido no grupo tratado com O 1 min (0,109 mm). Para FF, os valores de FS e FD para os grupos com fibras afastadas da base foram semelhantes ou superiores aos daqueles com fibras na base. O maior valor de FS foi obtido no grupo tratado com O 1 min (317,5 MPa) e o maior valor de FD foi obtido no grupo tratado com O 3 min (0,177 mm). O tratamento de plasma influenciou o FS e o FD. A posição de fibras, assim como o tratamento de plasma, afetaram as propriedades de flexão de um compósito reforçado com fibra.

Abstract: The aim of this study was to evaluate the effect of plasma treatment using argon and oxygen gases, combined with fiber position on flexural properties of a fiber-reinforced composite. Eleven groups were evaluated, a non-reinforced control group and 10 groups reinforced with InFibra, a woven polyethylene fiber, varying according to the plasma treatment and fiber position. The samples were prepared using a stainless steel two-piece matrix. The three point bending test was performed in an EMIC testing machine. Flexural strength (FS) and flexural deflection (FD) were calculated from initial (IF) and final (FF) failure. Data were evaluated statistically using Kruskal-Wallis and Mann-Whitney tests (p<0.05). For IF, in all groups with fibers placed on the base, the FS and FD values were significantly higher than those positioned away from the base. The highest value of FS was obtained in the group treated with O 3 min (296.2 MPa) and the highest value of FD was obtained in the group treated with 1 min (0.109 mm). For FF the FS and FD values obtained for the groups with fibers positioned away from the base were similar or higher than those placed on the base. The highest FS value was obtained in the group treated with 1 min (317.5 MPa) and the highest FD value was obtained in the group treated with O 3 min (0.177 mm). Plasma treatment influenced FS and FD. Fiber position and plasma treatment affected the flexural properties of a fiber-reinforced composite.

The objective of this work was to characterize the asphaltic cement penetration grade 30/45 (CAP 30/45) based on the morphology of nanostructures called "bee" structure observed and its modification when the binder was diluted in heptanes or toluene. The morphology of CAP30/45, toluene and heptane films was studied by Atomic Force Microscopy (AFM) tapping mode and showed typical "bee" structure in asphaltic cement films, but this structure is not visible on the other films. While, toluene completely dissolved the bees, films attacked with heptane still presented some structures left.

The development and maintenance of the sealing of the root canal system is the key to the success of root canal treatment. The resin-based adhesive material has the potential to reduce the microleakage of the root canal because of its adhesive properties and penetration into dentinal walls. Moreover, the irrigation protocols may have an influence on the adhesiveness of resin-based sealers to root dentin. Objective: The objective of the present study was to evaluate the effect of different irrigant protocols on coronal bacterial microleakage of gutta-percha/AH Plus and Resilon/Real Seal Self-etch systems. Material and Methods: One hundred ninety pre-molars were used. The teeth were divided into 18 experimental groups according to the irrigation protocols and filling materials used. The protocols used were: distilled water; sodium hypochlorite (NaOCl)+eDTA; NaOCl+H3PO4; NaOCl+eDTA+chlorhexidine (CHX); NaOCl+H3PO4+CHX; CHX+eDTA; CHX+ H3PO4; CHX+eDTA+CHX and CHX+H3PO4+CHX. Gutta-percha/AH Plus or Resilon/Real Seal Se were used as root-filling materials. The coronal microleakage was evaluated for 90 days against Enterococcus faecalis. Data were statistically analyzed using Kaplan-Meier survival test, Kruskal-Wallis and Mann-Whitney tests. Results: No significant difference was verified in the groups using chlorhexidine or sodium hypochlorite during the chemo-mechanical preparation followed by eDTA or phosphoric acid for smear layer removal. The same results were found for filling materials. However, the statistical analyses revealed that a final flush with 2% chlorhexidine reduced significantly the coronal microleakage. Conclusion: A final flush with 2% chlorhexidine after smear layer removal reduces coronal microleakage of teeth filled with gutta-percha/AH Plus or Resilon/Real Seal SE.

INTRODUÇÃO: O uso de irrigantes pode gerar alterações microestruturais na superfície dentinária, entre as quais alterações na rugosidade. Essas alterações podem influenciar o processo de união dos materiais obturadores à dentina. OBJETIVO: O objetivo do presente trabalho foi avaliar o efeito das soluções de EDTA, hipoclorito de sódio (NaOCl) e clorexidina, como irrigante final, na rugosidade da superfície dentinária. MATERIAL E MÉTODO: Foram utilizadas raízes distais de seis terceiros molares inferiores, que foram planificadas com o auxílio de disco de lixa e cortadas em segmentos, totalizando 18 amostras. A análise inicial foi realizada utilizando-se o perfilômetro Dektak. Foram realizadas cinco varreduras por amostra. Em seguida, as amostras foram irrigadas com NaOCl para simular o preparo químico-mecânico e lavadas com água destilada. Foram então divididas em seis grupos de acordo com o protocolo de irrigação final: Água destilada; NaOCl 5,25%; clorexidina 2%; EDTA17%; EDTA 17% + NaOCl 5,25%, e EDTA 17% + clorexidina 2%. Novamente, em cada amostra, foram realizadas cinco varreduras, totalizando 15 varreduras por grupo. Os dados foram analisados estatisticamente pelos testes de Kruskal-Wallis e Mann-Whitney (p<0,05). RESULTADO: Foi encontrada alteração significativa da rugosidade somente no grupo em que houve a combinação do agente quelante com o NaOCl. CONCLUSÃO: Os protocolos de irrigação final apresentam diferentes efeitos na rugosidade da superfície dentinária.

INTRODUCTION : The use of irrigators can create microstructural changes in the dentin surface, including changes in roughness. These changes may influence the bonding process of filling materials to dentin. OBJECTIVE: The aim of this study was to evaluate the effect of EDTA, sodium hypochlorite or chlorhexidine, as final irrigant, in the roughness of the dentin surface. MATERIAL AND METHOD: Distal root of 6 mandibular molars were used. The roots were flatted with the aid of sandpaper and segmented, totaling 18 samples. The initial analysis was performed by using Dektak profilometer. Five areas were scanned per sample. Then, the samples were irrigated with NaOCl to simulate the chemomechanical preparation and washed with distilled water. The segments were divided into six groups according to the final flush protocol: Distilled water, 5.25% NaOCl, 2% chlorhexidine, 17% EDTA, 17% EDTA+ 5.25% NaOCl, 17% EDTA+ 2% chlorhexidine. Once again, in each sample, five areas were scanned, totaling 15 scans per group. Data were statistically analyzed using Kruskal - Wallis and Mann -Whitney tests (p<0.05). RESULT: Significant changes in roughness were found only in the association of the chelating agent with NaOCl. CONCLUSION: The final irrigation protocols have different effects on surface roughness of dentin.

Nanostructured magnetic materials have great interest because of their applications in high-density magnetic information storage and for magnetic sensors. The electrodeposition of materials into porous alumina arrays is a suitable technique to produce nanomaterials, since highly ordered uniform nanomaterials can be obtained simply and cheaply. In this work, template-assisted Co nanowire arrays were prepared by electrodeposition into nanometer-sized pores of an alumite film using a two-electrode electrochemical cell. The Co nanowires were electrodeposited from a solution of 400 g/L of CoSO4.7H2O and 40 g/L of H3BO3. The morphology of the samples was investigated by means of TEM and AFM. The structural characteristic of the samples was examined using XRD, EDX and FTIR, which confirm the cobalt nanowire formation.