Abstract This study aimed to evaluate the microstructure formed after the chemical treatment of teeth, for the development of autogenous grafts from the demineralized dentin matrix (DDM) technique, in order to identify the most efficient demineralizing solution. The specimens, originating from the root and coronal portion, were submitted to ultrasonic cleaning and drying in an oven for 1h at 100 ºC. Then, the density was determined by Archimedes’ principle for each specimen, using distilled water as immersion liquid. The samples were separated into five groups: Control group: negative control, Distilled water;EDTA group: positive control, trisodium EDTA; NaOCl group: 2.5% sodium hypochlorite; HCl-0.6M group: 0.6M hydrochloric acid; and H2O2/H2SO4 group: hydrogen peroxide and sulfuric acid. Each specimen was immersed for 1h in the corresponding group descaling solution at 60 ºC. Subsequently, the mass loss and density of the treated specimens were determined by Archimedes’ principle. Ultimately, the specimens of each group were characterized by microtomography, Scanning Electron Microscopy, and Energy Dispersive Spectrometry X-ray (SEM-EDS). The results demonstrated that the H2O2/H2SO4 solution allowed the formation of interconnected micropores, suggesting better pore structures for application in scaffolds, when compared to the other studied solutions.

Resumo Este estudo teve como objetivo avaliar a microestrutura formada após o tratamento químico em dentes, para o desenvolvimento de enxertos autógenos a partir da técnica de matriz de dentina desmineralizada (DDM), a fim de identificar a solução desmineralizante mais eficiente. Os espécimes, provenientes da raiz e porção coronal, foram submetidos à limpeza ultrassônica e secagem em estufa por 1h a 100 ºC. Em seguida, a densidade foi determinada pelo princípio de Arquimedes para cada espécime, utilizando água destilada como líquido de imersão. As amostras foram separadas em cinco grupos: Controle: controle negativo, Água destilada; EDTA: controle positivo, EDTA trissódico; NaOCl: hipoclorito de sódio 2,5%; HCl-0.6M: ácido clorídrico 0,6M; e H2O2/H2SO4: peróxido de hidrogênio e ácido sulfúrico. Cada espécime foi imerso por 1h na solução descalcificante de grupo correspondente a 60 ºC. Posteriormente, a perda de massa e a densidade dos espécimes tratados foram determinadas pelo princípio de Arquimedes. Por fim, os espécimes de cada grupo foram caracterizados por microtomografia, microscopia eletrônica de varredura e espectrometria de energia dispersiva de raios-X (SEM-EDS). Os resultados demonstraram que a solução H2O2/H2SO4 permitiu a formação de microporos interligados, sugerindo melhores estruturas de poros para aplicação em scaffolds, quando comparada às demais soluções estudadas.

ABSTRACT The present work is a continuation of the research carried out in a previous work, with the aim of improving the production of Ti35Nb alloy by reducing the particle size of Ti (from 50–149 Μm to < 53 Μm) and Nb (from 31–500 Μm to < 62 Μm) powders. Micro (MI) and Macroporous (MA) Ti35Nb alloy samples were processed by powder metallurgy. Ammonium bicarbonate (AB) was utilized as pore former additive for processing MA samples. The powders were mixed, uniaxially pressed and then sintered at 1300 ºC for 2 hours under argon atmosphere. The samples were characterized by SEM/EDS, XRD, profilometry, and Vickers hardness test. The porosity levels were determined by geometric method, Archimedes’ principle and quantitative metallographic analysis. The results showed that the processing parameters used in this work successfully produced porous Ti35Nb alloys with completely stabilized β-Ti phase, indicating an enhancement in the methodology when compared with those reported in previous work. Smaller particle sizes influenced positively on the chemical-physical properties of MI and MA samples, since they demonstrated an improvement in the their characteristics, such as: more homogeneous microstructure; better particle consolidation; homogeneous elemental distribution with no relevant chemical contamination; porosity values in accordance with literature; presence of low amounts of titanium oxides on the surfaces which can improve the biocompatibility features; suitable surface roughness parameters for bone implant applications and favouring adhesion of bioceramic coatings; more uniform microhardness values for both samples which make the material with a further predictable mechanical behavior.

ABSTRACT Commercially dense pure titanium sheets and porous titanium samples processed by powder metallurgy were treated with a mixture consisting of equal volumes of H2SO4 and H2O2 for 2 or 4 hours. Characterization was performed by scanning electron microscopy, energy dispersive X-ray spectroscopy, confocal scanning optical microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. The analyses showed that the chemical patterning approach using a combination of concentrated acid and oxidant was able to generate a nanotexture on dense and porous titanium surfaces. In addition, the treated samples presented an oxide layer consisting predominantly of titanium dioxide with negative charge conferred by the presence of hydroxyl groups, which is an important factor that favors apatite nucleation and protein adsorption. It was also observed that oxide formation was more effective on porous samples than on dense samples, which can be explained by the higher surface area intrinsic to porous media. Finally, the findings indicated that both treatment times promoted similar modifications in surface properties, such as nanotexture and chemical composition, suggesting that the time of 2 hours were enough to induce the surface alterations at the nanoscale.

ABSTRACT Titanium-Niobium alloys have been studied for biomedical applications due to their satisfactory biocompatibility. In order to improve the long-term implantation, surface modification techniques have been developed to generate suitable topography, roughness, chemical composition, surface energy, etc. Considering this approach, the present work aimed to characterize Titanium-35Niobium (Ti-35Nb) surface modified by controlled chemical oxidation. Ti-35Nb (wt%) substrates were processed by powder metallurgy. The powders were mechanically mixed, uniaxially cold pressed and sintering at 1300ºC/2h. Then, the sintered substrates were immersed in a solution consisting of equal volumes of concentrated H2SO4 and 30% aqueous H2O2 for 4 hours at room temperature under continuous agitation. Sample characterizations were performed by scanning electron microscopy, profilometry, contact angle measurement, X-ray diffraction, and X-ray photoelectron spectroscopy. The results showed that the samples exhibited a microporous structure with micro-roughness on surface, and the β-Ti phase was stabilized by complete niobium atoms diffusion in titanium matrix. In addition, the chemical treatment successfully modified the Ti-35Nb surface with micropore formation and enhancement of hydrophilic feature and TiO2 and Nb2O5 layer, which can improve the biocompatibility of TiNb alloy implants.

RESUMO Neste trabalho foram preparadas dispersões aquosas de óxido de grafeno (GO) e óxido de grafeno reduzido (rGO), em diferentes tempos de oxidação, com o objetivo de verificar a influência do tempo de oxidação em relação às características das folhas (flakes) finais. As dispersões de GO foram preparadas pelo método de Hummers modificado utilizando os seguintes tempos de oxidação: 4 h; 1 dia; 3 dias; 7 dias e 10 dias. Em seguida, as dispersões de GO foram submetidas ao tratamento de redução com ácido ascórbico, obtendo-se o rGO. As caracterizações das amostras foram realizadas por meio das análises de espectroscopia Raman, espectroscopia de fotoelétrons excitados por raios X (XPS), microscopia eletrônica de varredura (MEV) e difração de raios X (DRX). A espectroscopia Raman mostrou a variação da relação de intensidade entre as bandas D e G (ID/IG) à medida que o tempo de oxidação foi aumentado. A análise de XPS exibiu a alteração dos percentuais de carbono (C) e oxigênio (O). Através de análise no MEV foi correlacionada a morfologia dos flakes com o aumento do tempo de oxidação. E por fim, com o auxílio de DRX, foi verificada a variação da distância interplanar.

ABSTRACT In this work aqueous dispersions of graphene oxide (GO) and reduced graphene oxide (rGO) were prepared in different oxidation times in order to verify the influence of the oxidation time on the characteristics of the final flakes. GO dispersions were prepared by the modified Hummers method, using the following oxidation times: 4 h; 1 day; 3 days; 7 days and 10 days. Afterwards the dispersions of GO were subjected to the reduction treatment with ascorbic acid, obtaining the rGO. Samples were characterized by Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and X-ray diffraction (XRD). Raman spectroscopy showed the variation of the intensity ratio between the D and G bands (ID / IG) as the oxidation time was increased. The XPS analysis indicated the alteration of the percentages of carbon (C) and oxygen (O). The SEM analysis correlated the morphology of the flakes with the increase of the oxidation time. Finally, with the aid of XRD, the variation of the interplanar distance was verified.

Biomaterials (composites and blends) play a major role in the health of modern society. This paper reports on the preparation and characterization of polyvinylidene fluoride (PVDF) and hydroxyapatite (HAP) composites, analyzing the incorporation of HAP in PVDF and investigating their mechanical properties and cytotoxicity (biocompatibility) for use in bone restoration and filling. The material was prepared in film form by the casting method. PVDF pellets were dissolved in dimethylacetamide (DMA), a HAP/DMA emulsion was prepared. The materials were mixed in proportions of 100/00, 90/10, 80/20, 70/30, 60/40, 50/50, 40/60, 30/70 in weight and left to dry in an oven, resulting in homogeneous, flexible films which were characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X ray diffractometry (XRD), contact angle measurement, and by mechanical and cytotoxicity tests.