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The influence of different surface treatments and ageing on the shear bond strength (SBS) of computer-aided design/computer-aided manufacturing (CAD/CAM) materials is still contentious. Therefore, this study evaluated the effect of surface treatments and ageing on the SBS of resin cement to polymer-infiltrated ceramic network (PICN) and zirconia-reinforced lithium silicate (ZLS) CAD/CAM materials. Specimens of PICN (n=10) and ZLS (n=10) were submitted to four surface treatment groups: 1) 5% hydrofluoric acid etching (HF) + silanisation (SI); 2) Air abrasion (AB)+HF+SI; 3) HF + universal adhesive (UA); 4) AB+HF+SI+UA. The treated specimens were bonded with resin cement cylinders and tested in SBS after 24 h and one year of water storage. Data were assessed by "analysis of variance" (ANOVA) and Tukey test (α=0.05) and failure modes were classified. No significant differences were observed among treatments at each evaluation time (p>0.05). SBS decreased after one year of storage, except for PICN treated with HF+UA (p=0.068). Air-abraded groups displayed a lower SBS reduction for ZLS. PICN and ZLS exhibited predominantly adhesive and mixed failures, but at one year, PICN cohesive failures increased. In conclusion, HF+UA is an effective surface treatment for PICN, while the combination AB+HF+SI+UA was more appropriate for ZLS. The water storage for one year reduced the SBS for most groups.

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A novel hybrid nanomaterial, nanoscale zero-valent iron (nZVI)-grafted imogolite nanotubes (Imo), was synthesized via a fast and straightforward chemical procedure. The as-obtained nanomaterial (Imo-nZVI) was characterized using transmission electron microscopy (TEM), electrophoretic mobility (EM), and vibrating sample magnetometry (VSM). The prepared Imo-nZVI was superparamagnetic at room temperature and could be easily separated by an external magnetic field. Sorption batch experiments were performed for single- and multicomponent systems and demonstrated that Hg2+ and Pb2+ could be quantitatively adsorbed at pH 3.0. For multicomponent systems, maximum adsorption capacities of 61.6 mg·g-1 and 76.9 mg·g-1 were obtained for Hg2+ and Pb2+ respectively. It was observed that the functional groups in Imo-nZVI interact preferentially with analytes according to the Misono softness parameter. The higher performance of Imo-nZVI compared with Imo and nZVI is related to the increased number of adsorption sites in the functionalized nanomaterial. The sorption equilibrium data obeyed the Langmuir model, while kinetic studies demonstrated that the sorption processes of Hg2+ and Pb2+ followed the pseudo-second-order model. This study suggests that the Imo-nZVI composite can be used as a promising sorbent to provide a simple and fast separation method to remove Hg and Pb ions from contaminated water.

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Rare diseases affect a small part of the population, and the most affected are children. Because of the low availability of patients for testing, the pharmaceutical industry cannot develop drugs for the diagnosis of many of these orphan diseases. In this sense, the use of benzothiazole compounds that are highly selective and can act as spectroscopy probes, especially the compound 2-(4'-aminophenyl)benzothiazole (ABT), has been highlighted. This article reports the design of potential contrast agents based on ABT and iron to develop a new material with an efficient mechanism to raise the relaxation rate, facilitating diagnosis. The ABT/δ-FeOOH hybrid material was prepared by grafting (N-(4'-aminophenyl) benzothiazole-2-bromoacetamide) on the surface of the iron oxyhydroxide particles. FTIR spectra confirmed the material formations of the hybrid material ABT/δ-FeOOH. SEM analysis checked the covering of nanoflakes' surfaces in relation to the morphology of the samples. The theoretical calculations test a better binding mode of compound with iron oxyhydroxide. Theoretical findings show the radical capture mechanism in the stabilization of this new material. In this context, Fe3+ ions are an electron acceptor from the organic phase.

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This paper presents the synthesis of a hybrid material through the use of natural pozzolan and titanium(IV) isopropoxide using the sol-gel method and its application in the photocatalytic hexavalent chromium reduction. The characterization data indicated a mesoporous material possessing a surface area of 271.7 m2 g-1. The morphology studies (SEM and TEM) showed nanosheet hybrid structures. The analysis of DRUV, FTIR, XRD, and Mössbauer spectroscopy provides a different electronic structure of the synthetized material when compared with the originals, proving the hybridization process between pozzolan and titanium(IV) isopropoxide. The photocatalytic reduction of Cr(VI) to Cr(III) using the hybrid material showed a better performance than conventional photocatalysts (precursor and TiO2-P25). Operational conditions such as chromium initial concentration (0.02-0.20 mM), solution pH (3-6), and type of scavenger (citric or tartaric acid) were evaluated in order to determine the best experimental conditions for the Cr(VI) photoreduction. At their optimum (catalyst load of 15 mg L-1, tartaric acid as scavenger, [scavenger]0/[Cr(VI)]0 M ratio = 3:1, pH 3, and 25 °C), the total photoreduction of 0.20 mM Cr(VI) was achieved in 180 min. The novel hybrid materials synthesized from pozzolan and titanium(IV) isopropoxide showed to be a potential catalyst for the Cr(VI) reduction in aqueous solution. Graphical abstract.

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Herein, we report the preparation of an organic-inorganic hybrid hydrogel architecture using vinyl alginate and UiO-66 MOFs (metal-organic frameworks) modified with acrylic acid (AA) UiO-66AA. UiO-66 MOFs with different crystal sizes (600, 1500, and 2500 nm) were synthesized and the effect on the mechanical and transport properties of the resulting materials, such as water absorption capacity and drug release, were evaluated. HydroMOF showed higher water absorption capacity than the pure hydrogel and enhanced mechanical properties, which depend on crystal size and the amount of UiO-66AA MOF used. The initial release rate of drug (burst release) from hydroMOFs was lower when small-sized crystals or a small amount of large-sized crystals were used; thus these are essential in changing half-life values of release rates. Finally, the cytotoxicity screening successfully showed that hydroMOFs are promising biocompatible compounds proven to have the advantages of minimized burst release and mechanical robustness.

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Caffeic acid (CA) molecules were immobilized in a layered inorganic host matrix based on zinc hydroxide structures with different starting interlayer anions, nitrate, and acetate. The chemical composition, structure, thermal stability, morphology, and surface of the host matrices and hybrid compounds were analyzed by X-ray diffraction (XRD), themogravimetric/differencial thermal analysis (TG/DTA), Fourier transform infrarred spectroscopy (FT-IR), scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS). Additionally, the surface charge of the materials was investigated using zeta potential at pH ~7. The results show an influence of the surface charge on the chemical, interaction, and structure of the resulting hybrid materials as a function of the starting layered structures. An expansion of the basal spacing to 10.20 Å for zinc hydroxide nitrate (ZHN), and a shrinkage to 10.37 Å for zinc hydroxide acetate (ZHA). These results suggest that the CA lies with a tilt angle in the interlayer region of the inorganic host matrix. The immobilization of CA is favored in ZHN, with respect to ZHA, because a single-layered phase was identified. A higher thermal stability at 65 °C was observed for ZHN-CA than for ZHA-CA. The evaluation of the release behavior showed a higher percentage of CA released from ZHN than ZHA, and the release mechanism was described by the Elovich model. The hybrid materials show potential characteristics for use as bioactive delivery systems.

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A glassy carbon electrode was modified with a TiO2-gold nanoparticle hybrid integrated with multi-walled carbon nanotubes in a dihexadecylphosphate film (TiO2-Au NP-MWCNT-DHP/GCE) and applied to amperometric determination of ascorbic acid (AA). The modified sensor displays fast charge transfer and shows an irreversible anodic behavior for AA by cyclic voltammetry. Under optimal experimental conditions and using amperometry at 0.4 V, the analytical curve presented a statistical linear concentration range for AA from 5.0 to 51 µmol L-1, with a limit of detection of 1.2 µmol L-1. The electrode was successfully applied to the determination of AA in pharmaceutical and fruit juice without the need for major pretreatment of samples. Graphical abstract Schematic of a new sensing platform for ascorbic acid (AA). It is based on a glassy carbon electrode (GCE) modified with TiO2-Au nanoparticles integrated into carbon nanotubes in a dihexadecylphosphate film. The sensor was applied to amperometric determination of AA in juice and pharmaceutical samples.

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Cellulose nanowhiskers (CNWs) with different surface composition were used to generate the biomimetic growth hydroxyapatite (HAp). Hybrids materials primarily consist of CNWs with HAp content below 24%. CNWs were produced by different inorganic acid hydrolyses to generate cellulose particles with surface groups to induce HAp mineralization. In the present study, we evaluate the use of CNWs prepared from hydrochloric acid, sulfuric acid and phosphoric acid. HAp growth was obtained from the biomimetic method using a simulated body fluid concentration of 1.5M (SBF). The sulfonate and phosphonate groups on the CNW surface have a direct impact on the nucleation and growth of HAp. HAp/CNW were also compared with the physical mixture method using HAp nanoparticles prepared by chemical precipitation. The bioactivity and biocompatibility of the hybrid materials were assessed by cell viability studies using fibroblast cells (L929). The materials obtained from the biomimetic method have superior biocompatibility/bioactivity compared to the material synthesized by the wet chemical precipitation method with an incubation period of 24h.

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Organically modified vermiculites were synthesized by previous silylation of three leached vermiculites, V0.3Cl, V0.5Cl and V0.8Cl, under anhydrous conditions following reaction with imidazole (Im), which acted as chelating agent for copper retention. Elemental analysis, X-ray diffraction, infrared spectroscopy, scanning electronic microscopy, transmission electron microscopy, (29)Si and (13)C NMR and nitrogen adsorption/desorption measurements were used to characterize pristine, leached and organofunctionalized solids. X-ray photoelectron spectroscopy (XPS) was used to evaluate the surface after copper sorption. Parameters such as contact time, pH and initial cation concentration for the adsorption of Cu(II) ions were investigated. The adsorption equilibrium data were fitted using the Langmuir isotherm model and the monolayer adsorption capacities were 2.38, 2.52 and 2.69mmolg(-1) for V0.5Cl-Im, V0.3Cl-Im and V0.8Cl-Im, respectively, at pH 6.0 and 298K for a time reaction of 80min. The sorption rates were described by pseudo-second-order kinetics. The chloropropyl imidazole vermiculites are promising adsorbents for the rapid removal of Cu(II) ions from aqueous solution.

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In this paper, we report the synthesis of polycaprolactone (PCL) based hybrid materials containing hydrophilic domains composed of N-vinylpyrrolidone (VP), and γ-methacryloxypropyltrimethoxysilane (MPS). The hybrid materials were obtained by RAFT copolymerization of N-vinylpyrrolidone and MPS using a pre-formed dixanthate-end-functionalized PCL as macro-chain transfer agent, followed by a post-reaction crosslinking step. The composition of the samples was determined by elemental and thermogravimetric analyses. Differential scanning calorimetry and X-ray diffraction indicated that the crystallinity of PCL decreases in the presence of the hydrophilic domains. Scanning electron microscopy images revealed that the samples present an interconnected porous structure on the swelling. Compared to PCL, the hybrid materials presented low water contact angle values and higher elastic modulus. These materials showed controlled release of diclofenac, and biocompatibility with human periodontal ligament fibroblasts.

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Poly [Ni-Protoporphyrin] film (pNiPP), containing multiwall carbon nanotubes (MWCNT) was used to cover a glassy carbon electrode. The hybrid material (pNiPP/MWCNT) successfully combines the permselectivity of pNiPP with the high conductivity of MWCNT. The modified electrode was used to perform amperometric detection of long chain aliphatic amines (LCAA) in order to prevent the passivation effect of the aliphatic chain. Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) demonstrated that the pNiPP/MWCNT facilitates the electron transfer reaction. The charge transfer resistance (Rct) values were significantly lower by up to one order of magnitude compared to the bare electrode. Differential pulse polarography (DPP) showed a marked decrease of the overpotential generated by the aliphatic chain. The calibration of the amperometric peak area vs. concentrations of derivatized LCAA exhibits a linear response within the range of 0.018 and 28 µM and correlation coefficient (R(2)) higher than 0.999 (n=5). The quantitation limit of the pNiPP/MWCNT electrode is about 400 times lower than the UV-visible detection. RSD of 7.2%, 5.8%, 2.5% and 2.3% was obtained for concentrations of 0.028, 0.28, 2.8 and 28 µM of ferrocenyl octadecylamine. A solution of sphingosine, 0.23 µM, was exclusively detected with HPLC-ECD with pNiPP/MWCNT electrode.

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Hybrid organic-inorganic material containing Laponite clay and ionic liquids forming cations have been prepared and characterized by FT-Raman spectroscopy, X-ray diffraction, and thermal analysis. The effect of varying the length of the alkyl side chain and conformations of cations has been investigated by using different ionic liquids based on piperidinium and imidazolium cations. The structure of the N,N-butyl-methyl-piperidinium cation and the assignment of its vibrational spectrum have been further elucidated by quantum chemistry calculations. The X-ray data indicate that the organic cations are intercalated parallel to the layers of the clay. Comparison of Raman spectra of pure ionic liquids with different anions and the resulting solid hybrid materials in which the organic cations have been intercalated into the clay characterizes the local environment experienced by the cations in the hybrid materials. The Raman spectra of hybrid materials suggest that the local environment of all confined cations, in spite of this diversity in properties, resembles the liquid state of ionic liquids with a relatively disordered structure.

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