ABSTRACT Currently, the titanium substrate is one of the most important metallic biomaterials with application in orthopedics, dentistry, fracture fixation and knee and hip arthroplasty. Despite all these attractive properties, its biological inertia and low bactericidal capacity ends up limiting its osseointegration. In this sense, TiO2 and TiO2(MgO) coatings are performed to improve titanium characteristics, such as corrosion resistance. The objectives of this study were to analyze the corrosion resistance of titanium oxide and titanium oxide with addition of magnesium, topographies, morphologies and crystallinity on a titanium substrate through electrodeposition with constant current. Electrodepositions were performed on a three-electrode system, with titanium working electrode, Ag/AgCl as reference electrode and a platinum counter electrode in a potentiostat, and constant currents of 1.0 mA/cm2 were used for all processes. Characterizations by scanning electron microscopy (SEM), atomic force microscopy (AFM), confocal microscopy, X-Ray diffraction (XRD) and potentiodynamic polarization were used. Topography and morphology analyze indicated a change in roughness (Ra) and all demonstrated a uniform surface. The XRD analyzes indicated only metallic titanium, but all of them had a difference in the FWHM, indicating possible amorphous phases or interstitial Mg, also causing a variation in the height of the peaks. Finally, the potentiodynamic polarization indicated that the coating with TiO2 there was an improvement of 37.90% and the TiO2 with addition of magnesium there was a loss of 13.43%. Therefore, the coatings caused changes in roughness, morphologies, crystalline networks and anticorrosive properties, thus enabling the modulation of the desired properties according to the oxidation environment used.

RESUMO Atualmente, o substrato de titânio é um dos mais importantes biomateriais metálicos com aplicação em ortopedia, odontologia, fixação de fraturas e artroplastia de joelho e quadril. Apesar de todas estas propriedades atrativas, sua inércia biológica e baixa capacidade bactericida acaba limitando sua osseointegração. Neste sentido, revestimentos de TiO2 e TiO2(MgO) são realizados para aprimorar as características do titânio, como a resistência à corrosão. Os objetivos deste estudo foram analisar a resistência à corrosão do óxido de titânio e óxido de titânio com adição de magnésio, topografias, morfologias e cristalinidade em um substrato de titânio através da eletrodeposição com corrente constante. As eletrodeposições foram realizadas em um sistema de três eletrodos, sendo o titânio eletrodo de trabalho, Ag/AgCl como eletrodo de referência e um contra eletrodo de platina em um potenciostato e foram utilizadas correntes constantes de 1,0 mA/cm2 para todos os processos. Foram utilizadas as caracterizações por microscopia eletrônica de varredura (MEV), microscopia de força atômica (MFA), microscopia confocal, difração de raios X (DRX) e polarização potenciodinâmica. As análises de topografia e morfologia indicaram uma alteração nas rugosidades (Ra) e todas demonstraram uma superfície uniforme. As análises de DRX indicaram apenas o titânio metálico, porém todas tiveram uma diferença no FWHM, indicando possíveis fases amorfas ou Mg intersticial, causando também uma variação na altura dos picos. Por fim, a polarização potenciodinâmica indicou que o revestimento com TiO2 houve uma melhora de 37,90% e o TiO2 com adição de magnésio houve uma perda de 13,43%. Portanto, os revestimentos causaram alterações nas rugosidades, morfologias, redes cristalinas e nas propriedades anticorrosivas, possibilitando assim a modulação das propriedades desejadas de acordo com o ambiente de oxidação utilizado.

Abstract This study aimed to investigate whether GSK-3 inhibition (CHIR99021) effectively promoted mineralization by cementoblasts (OCCM-30). OCCM-30 cells were used and treated with different concentrations of CHIR99021 (2.5, 5, and 10 mM). Experiments included proliferation and viability, cellular metabolic activity, gene expression, and mineral nodule formation by Xylene Orange at the experimental time points. In general, CHIR99021 did not significantly affect OCCM-30 viability and cell metabolism (MTT assay) (p > 0.05), but increased OCCM-30 proliferation at 2.5 mM on days 2 and 4 (p < 0.05). Data analysis further showed that inhibition of GSK-3 resulted in increased transcript levels of Axin2 in OCCM-30 cells starting as early as 4 h, and regulated the expression of key bone markers including alkaline phosphatase (Alp), runt-related transcription factor 2 (Runx-2), osteocalcin (Ocn), and osterix (Osx). In addition, CHIR99021 led to an enhanced mineral nodule formation in vitro under both osteogenic and non-osteogenic conditions as early as 5 days after treatment. Altogether, the results of the current study suggest that inhibition of GSK-3 has the potential to promote cementoblast differentiation leading to increased mineral deposition in vitro.

Abstract Titanium dioxide nanotubes (TiO2-nts) were incorporated into a glass ionomer cement (GIC) with improved mechanical properties and antibacterial activity. The aims of the present in vitro study were to define the elemental characterization, aluminum (Al) release rate, and initial working time for GIC reinforced with TiO2-nts, in an experimental caries model. TiO2-nts were incorporated into GIC powder components at 5% by weight, and compared with unblended GIC. Experimental approaches used energy-dispersive spectrometry (EDS), atomic absorption spectrophotometry (AAS), and brightness loss to define surface element properties, Al release rates, and initial working time, respectively. Statistical analysis was performed by 2-way ANOVA, Tukey’s test, generalized linear models, and Student’s t test (a = 0.05). EDS data analysis revealed that TiO2-nts incorporated into GIC had no significant impact on the typical elemental composition of GICs in an in vitro caries model. Regarding the demineralizing solution, GIC with TiO2-nt significantly decreased the Al release rate, compared with the control group (p < 0.0001). Moreover, TiO2-nt incorporated into GIC did not alter the initial working time of the material (p > 0.05). These findings add information to our scientific body of knowledge concerning the potential impact of TiO2-nt on the performance of conventional GICs.

Abstract This in vitro study evaluated the impact of TiO2 nanotubes (n-TiO2) incorporated into glass ionomer cement (GIC) on Streptococcus mutans (S. mutans) characteristics at cellular and molecular levels. n-TiO2, synthesized by the alkaline method (20 nm in size), was added to Ketac Molar EasyMix® at 0%, 3%, 5%, and 7% by weight. S. mutans strains were cultured on GIC disks with addition or not of n-TiO2 for 1, 3, and 7 days and the following parameters were assessed: inhibition halo (mm) (n=3/group); cell viability (live/dead) (n=5/group); cell morphology (SEM) (n=3/group); and gene expression by real-time PCR (vicR, covR, gtfB, gtfC, and gtfD) (n=6/group). The data were analyzed by the Kruskal-Wallis test, repeated-measures ANOVA or two-way ANOVA, and Tukey’s and Dunn’s post-hoc tests (α=0.05). The agar diffusion test showed a higher antibacterial property for 5% n-TiO2 compared with 3% and 7% (p<0.05) with no effect of time (1, 3, and 7 days). The cell number was significantly affected by all n-TiO2 groups, while viability was mostly affected by 3% and 5% n-TiO2, which also affected cell morphology and organization. Real-time PCR demonstrated that n-TiO2 reduced the expression of covR when compared with GIC with no n-TiO2 (p<0.05), with no effect of time, except for 3% n-TiO2 on vicR expression. Within-group and between-group analyses revealed n-TiO2 did not affect mRNA levels of gtfB, gtfC, and gtfD (p>0.05). Incorporation of n-TiO2 at 3% and 5% potentially affected S. mutans viability and the expression of key genes for bacterial survival and growth, improving the anticariogenic properties of GIC.

The controlled release of Salicylic Acid (SA) influences the concentration and collateral effects of the drug. This release refers to the matrix in which the SA is incorporated. Among the matrices, Fe3O4 nanoparticles (NPs) stand out, for transporting drugs to specific sites. The functionalization of Fe3O4 by bovine serum albumin (BSA) can improve colloidal and chemical stability, in addition to increasing interactions with drugs. Thus, understanding the release kinetics of the AS incorporated in Fe3O4-BSA is essential to improve the controlled release. The study aimed the synthesis, characterization and release of the SA into the Fe3O4-BSA NPs. The results showed the functionalization of the Fe3O4-BSA NPs was effective and the average size was below 30 nm. The NPs showed colloidal stability above the pH of 7.5 which can be used as a drug carrier in blood plasma. Drug encapsulation into the NPs system was efficient (~91%) with about 30% of drug loading capability. The kinetic results showed the SA release mechanism was controlled by diffusion. The conclusion is that the incorporation of SA in Fe3O4-BSA NPs led to a release of SA in the first six hours, reaching equilibrium at 0.265 mg mL-1; and 1.83 mg.

Abstract Titanium dioxide nanotubes are nanostructures that can accelerate the oxidation reaction of bleaching procedures and promote a more effective whitening effect. Objective This study evaluated physicochemical properties of bleaching agents incorporated with titanium dioxide (TiO2) nanotubes, and the effects on tooth color change at different periods. Methodology 40 premolars were treated according to the following groups (n=10): CP - 10% carbamide peroxide (1 hour daily/21 days); CPN - CP incorporated into TiO2; HP - 40% hydrogen peroxide (three 40-minute sessions/7 days apart); HPN - HP incorporated into TiO2. Color shade was evaluated at five different periods (baseline, after 7, 14 and 21 days of bleaching, and 7 days after end of treatment) according to Vita Classical, CIELab and CIEDE2000 scales. Mean particle size (P), polydispersity (PO) and zeta potential (ZP) were evaluated using dynamic light scattering. Data on the different variables were analyzed by mixed model tests for measures repeated in time (ZP e L*), generalized linear models for measures repeated in time (P, PO, Vita Classical and b*), and Friedman and Mann-Whitney tests (a* and color change/ΔE and ΔE00). Results CP and CPN presented higher P, higher PO and lower ZP than HP and HPN (p≤0.05). All groups showed a significant decrease in Vita Classical color scores after 7 days of bleaching (p<0.05), and HPN presented a greater significant reduction than the other groups. L* increased in TiO2 presence, in all groups, without any differences (p>0.05) in bleaching time. A significant reduction occurred in the a* and b* values for all the groups, and HPN presented lower a* and b* values (p<0.05) than CPN. ΔE was clinically noticeable after 7 days, in all groups, and all groups resulted in a perceptible color change according to ΔE00. Conclusion TiO2 did not influence physicochemical properties of the bleaching agents. HPN presented more effective tooth bleaching than CPN.

Abstract Objective This study aims to evaluate the effect of sonochemical treatment on the surface of yttria-stabilized tetragonal zirconia (Y-TZP) before and after the final sintering. Material and Methods Twenty-eight Y-TZP discs were divided into four groups (n=7), according to surface treatment: PRE: pre-sintering sonication with 30% nominal power for 15 min; POS: post-sintering sonication with 30% nominal power for 15 min; JAT: air abrasion with 50-μm alumina particles; and CON: control group with no treatment. The POS and JAT groups were sintered before sonication and the PRE group after sonication. Surface roughness was analyzed using confocal microscopy, after which resin cement cylinders were placed on the surface of the Y-TZP discs and subjected to mechanical microshear bond strength test until fracture. Surface roughness and microshear bond strength values underwent ANOVA and the Tukey tests. Results The surface roughness values for the PRE group (299.91 nm) and the POS group (291.23 nm) were not significantly different (p≥0.05), statistically, and the surface roughness value of the JAT group (925.21 nm) was higher than those of PRE and POS (p=0.007) groups. The mechanical microshear bond strength test showed that there was no statistically significant difference between the groups (p=0.08). Conclusions Therefore, the results showed that sonochemical treatment modifies the Y-TZP surface and is similar to the well-established sandblasting surface treatment regarding the strength of the bond with the resin cement.

Abstract Sandblasting is a common method to try to improve the Y-TZP/veneer bond strength of dental prostheses, however, it may put stress on zirconia surfaces and could accelerate the t→m phase transformation. Y-TZP sandblasting before sintering could be an alternative to improve surface roughness and bonding strength of veneering ceramic. Objectives. The aim of this study was to analyze the effect of Y-TZP pre-sintering sandblasting on surface roughness, phase transformation, and the Y-TZP/veneer shear bond strength. Material and Methods. The Y-TZP specimen surface underwent sandblasting with aluminum oxide (50 μm) pre-sintering (Z-PRE) and post-sintering (Z-POS). Z-CTR was not subjected to surface treatment. After ceramic veneer application, the specimens were subjected to shear bond testing. Surface roughness was analyzed by confocal microscopy. Y-TZP monoclinic and tetragonal phases were evaluated by micro-Raman spectroscopy. Shear bond strength and surface roughness data were analyzed by One-way ANOVA and Tukey tests (α=0.05). Differences in the wave numbers and the broadening bands of the Raman spectra were compared among groups. Results. Z-POS (9.73±5.36 MPa) and Z-PRE (7.94±2.52 MPa) showed the highest bond strength, significantly higher than that of Z-CTR (5.54±2.14 MPa). The Ra of Z-PRE (1.59±0.23 µm) was much greater and significantly different from that of Z-CTR (0.29±0.05 µm) and Z-POS (0.77±0.13 µm). All groups showed bands typical of the tetragonal (T) and monoclinic (M) phases. Y-TZP sandblasting before sintering resulted in rougher surfaces but did not increase the shear bond strength compared to post-sintering and increased surface defects. Conclusions. Surface treatment with Al3O2, regardless of the moment and application, improves the results of Y-TZP/veneer bonding and is not a specific cause of t→m transformation.

In this work, the surface and electrical characteristics ZnO:Al thin films deposited by RF magnetron sputtering onto glass substrates have been investigated. Analysis of surface morphologies revealed two growth stages. In the first stage, up to thicknesses of 100 nm, the films show surface structures with a granular form without preferential orientation. Beyond thicknesses of 100 nm, however, the grain structures increase in size and height, producing a pyramidal form and preferred orientation along the c-axis. The XRD results show that the films have a preferred orientation in the (002) plane. Furthermore, with the evolution of the film thickness the electrical resistivity decreases to a minimum of 1.6 × 10- 3 Ω cm for the film of 465 nm thickness. The doping with aluminum atoms produces an increase in concentration of charge carriers to around 8.8 × 10(19) cm- 3. All films exhibit high optical transmittance (above 85%) in the visible region.

The performance of advanced electronic ceramics is directly related to the synthesis route employed. Sol-gel methods are widely used for this purpose. However, the physicochemical intermediate steps are still not well understood. Better understanding and control of these processes can improve the final quality of samples. In this work, we studied theoretically the formation of metal complexes between citric acid and lithium or barium metal cations with different citric acid/metal proportions, using Density Functional Theory electronic structure calculations. Infrared and Raman scattering spectra were simulated for the more stable geometric configurations. Using this methodology, we identified some features of complexes formed in the synthesis process. Our results show that the complexes can be distinguished by changes in the bands assigned to C=O, COH-, and COO- group vibrations. An estimate of the most stable complexes is made based on total energy.

La variedad de aplicaciones tecnológicas relacionadas a los dispositivos basados en óxidos semiconductores nanoestructurados ha despertado un gran interés en la comunidad científica, haciendo con que los estudios relacionados a estos materiales han aumentado en los últimos años. Entre estos materiales, se encuentra el óxido de zinc (ZnO), que presenta aplicaciones en las más diversas áreas, desde diodos emisores de luz (LEDs) a los dispositivos fotovoltaicos en células solares. Con el conocimiento de que las propiedades químicas y físicas que confieren a estos materiales las posibilidades de aplicación en dispositivos tecnológicos son fuertemente dependientes de las rutas de síntesis empleadas para la obtención de los mismos, presentamos en este trabajo una investigación con respecto de las modificaciones morfológicas ocurridas en partículas de ZnO, cuando el mismo es expuesto a un tratamiento sonoquímico, además de las influencias de los parámetros relacionados a éste método de síntesis en la obtención de este material. Para analizar los parámetros presentados anteriormente, tres muestras fueron preparadas, dos de ellas manteniendo la amplitud y variando el tiempo de sonicación y otra manteniendo el tiempo y variando la amplitud de sonicación, durante el tratamiento sonoquímico. El análisis de los resultados obtenidos indica que el tratamiento sonoquímico conduce a modificaciones morfológicas superficiales en las partículas de ZnO, además estas modificaciones se presentaron más evidentes cuando una mayor amplitud y un mayor tiempo de sonicación fueron utilizados en la síntesis de las muestras.

A variety of technological applications related to oxide semiconductor-based devices have attracted great interest among the scientific community, leading to an increase in studies of these materials during the last years. Among such materials, zinc oxide (ZnO) has applications in several areas, from light- emitting diodes (LEDs) to photovoltaic devices in solar cells. Considering the physical and chemical properties conferred to these materials, the possibilities of application in technological devices depend greatly on the synthesis routes employed. Accordingly, we investigated the morphological modifications in ZnO particles when subjected to sonochemical treatment and the influence of related synthesis method parameters, such as the time and amplitude of sonication. To analyze such effects, four samples were prepared with different sonochemical treatment conditions: in two, the amplitude of sonication was kept constant while varying the time of sonication, and in the other two, the time was kept constant while varying the amplitude. The analysis of the results obtained indicated that sonochemical treatment led to superficial morphological modifications in ZnO particles. Furthermore, these modifications became more apparent when higher amplitude and longer time of sonication were employed in sample synthesis.

In this paper, it is reported the growth of La0.7Ca0.3MnO3±δ films using a chemical solution deposition method (CSD) by the spin-coating technique. Such solution was prepared through a route based on modified polymeric precursor method. Spin-coating deposition on different ceramic substrates was performed and analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The magnetic response of the prepared specimens was studied using a SQUID magnetometer. The obtained results indicated uniform deposition on SrTiO3 and LaAlO3 substrates with similar characteristics. Furthermore, significant differences were detected in the Mn3+/Mn4+ valence ratio and a corresponding diverse magnetic response was observed. The sample prepared on SrTiO3 and LaAlO3 presented a critical temperature around 270 K as expected.

The carbon dioxide reforming of methane was carried out over nickel catalysts supported on the gamma-Al2O3/CeO2 system prepared by wet impregnation. With the increase of the CeO2 weight in the catalyst, a higher stability was observed in the catalytic activity, together with an excellent resistance to carbon deposition and a better Ni dispersion. The catalysts were characterized by means of surface area measurements, TPR, H2 chemisorption, XRD, SEM, EDX, XPS and TEM. An interaction between Ni and CeO2 was observed to the Ni/CeO2 sample after activation in a H2 atmosphere above 300 ºC. Such behavior has a significantly influence on the catalytic activity.

Nickel nanoparticles supported on amorphous silica ceramic matrix were synthesized by the polymeric precursor method. The nanostructure was characterized by NMR, BET, XRD, SEM, TEM, and flame atomic absorption spectrometry techniques. It was observed a dependence of the crystallite size on the thermal annealing, under a N2 atmosphere. The materials presented a high catalytic activity and selectivity upon the beta-pinene hydrogenation reaction. The magnetic hystereses were also correlated with the morphology of the processed material.