Desenvolvimento de revestimentos siloxano-PMMA reforçados por nanotubos de carbono, óxido de grafite e óxido de grafite reduzido para aplicações anticorrosivas

Pós-graduação em Química - IQ

Effect of random/aligned nylon-6/MWCNT fibers on dental resin composite reinforcement

The aims of this study were (1) to synthesize and characterize random and aligned nanocomposite fibers of multi-walled carbon nanotubes (MWCNT)/nylon-6 and (2) to determine their reinforcing effects on the flexural strength of a dental resin composite.Nylon-6 was dissolved in hexafluoropropanol (10 wt%), followed by the addition of MWCNT (hereafter referred to as nanotubes) at two distinct concentrations (i.e., 0.5 or 1.5 wt%). Neat nylon-6 fibers (without nanotubes) were also prepared. The solutions were electrospun using parameters under low- (120 rpm) or high-speed (6000 rpm) mandrel rotation to collect random and aligned fibers, respectively. The processed fiber mats were characterized by scanning (SEM) and transmission (TEM) electron microscopies, as well as by uni-axial tensile testing. To determine the reinforcing effects on the flexural strength of a dental resin composite, bar-shaped (20 x 2 x 2 mm(3)) resin composite specimens were prepared by first placing one increment of the composite, followed by one strip of the mat, and one last increment of composite. Non-reinforced composite specimens were used as the control. The specimens were then evaluated using flexural strength testing. SEM was done on the fractured surfaces. The data were analyzed using ANOVA and the Tukey's test (alpha=5%).Nanotubes were successfully incorporated into the nylon-6 fibers. Aligned and random fibers were obtained using high- and low-speed electrospinning, respectively, where the former were significantly (p<0.001) stronger than the latter, regardless of the nanotubes'presence. Indeed, the dental resin composite tested was significantly reinforced when combined with nylon-6 fibrous mats composed of aligned fibers (with or without nanotubes) or random fibers incorporated with nanotubes at 0.5 wt%. (C) 2015 Elsevier Ltd. All rights reserved.

Estudo da cinética de decomposição de compósitos nanoestruturados de poli (sulfeto de fenileno) reforçados com nanotubos de carbono

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Renewable nanocomposite layer-by-layer assembled catalytic interfaces for biosensing applications

A novel, easily renewable nanocomposite interface based on layer-by-layer (LbL) assembled cationic/anionic layers of carbon nanotubes customized with biopolymers is reported. A simple approach is proposed to fabricate a nanoscale structure composed of alternating layers of oxidized multiwalled carbon nanotubes upon which is immobilized either the cationic enzyme organophosphorus hydrolase (OPH; MWNT−OPH) or the anionic DNA (MWNT−DNA). The presence of carbon nanotubes with large surface area, high aspect ratio and excellent conductivity provides reliable immobilization of enzyme at the interface and promotes better electron transfer rates. The oxidized MWNTs were characterized by thermogravimetric analysis and Raman spectroscopy. Fourier transform infrared spectroscopy showed the surface functionalization of the MWNTs and successful immobilization of OPH on the MWNTs. Scanning electron microscopy images revealed that MWNTs were shortened during sonication and that LbL of the MWNT/biopolymer conjugates resulted in a continuous surface with a layered structure. The catalytic activity of the biopolymer layers was characterized using absorption spectroscopy and electrochemical analysis. Experimental results show that this approach yields an easily fabricated catalytic multilayer with well-defined structures and properties for biosensing applications whose interface can be reactivated via a simple procedure. In addition, this approach results in a biosensor with excellent sensitivity, a reliable calibration profile, and stable electrochemical response.

Efeito de diferentes cargas orgânicas em cimentos resinosos experimentais

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Obtenção de nanofibras de carbono a partir do processo de eletrofiação

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Determinação de açucares em bagaço de palha de cana-de-açúcar por cromatografia líquida de alta eficiência com detecção eletroquímica utilizando eletrodos de nanotubos modificados com óxidos metálicos

Pós-graduação em Química - IQ

Influência da incorporação de nanofibras de poliamida 6 com e sem nanotubos de carbono como reforço de prótese parcial fixa adesiva

The aim of this study was to evaluate the behavior of reinforced composites with polyamide 6 fibers aligned (6000 rpm) and alignment (120 rpm) with or without CNT using the flexural strength test. After preparation of nanofibers aligned nylon 6 (6000 rpm) and alignment (120 rpm) with and without incorporation of nanotube carbon by the method of electrospinning, were performed one control group (n = 10) and 4 experimental groups (n = 40) G1: Control (just resin Charisma - Heraeus Kulzer) ;G2 Resin + N6 aligned (6000 rpm) + CNT; G3:Resin + N6 alignment (120 rpm) + CNT; G4: Resin + aligned ( 6000 rpm) N6. G5: Resin + N6 alignment (120 rpm). The fibers were cut to the dimensions of 0,3 x 15 mm and were applied an adhesive at the surface (Single Bond 2) for 5 min and cured. In the matrix, was added resin in the proximal box (Charisma A2, Heraeus Kulzer) and cured for 40 s. (power 1100 mW / cm²). A first layer of resin and on the resin was deposited. The resin layers specimens were light irradiated with three overlapping exposures delivered. For each resin layer were light irradiated for 40 sec. The samples were tested with a cross-speed of 1 mm / min, and a 50 Kgf at Universal testing machine (EMIC mod.DL2000). The Dunnet test showed that only the nanotube group was significantly different from the control group. The ANOVA two-way indicates that the nanotube factor was statistically significant (p < 0.05) and there is no interaction between factors and orientation nanotube. The presence of nanotube showed lower fracture resistance values for aligned and unaligned groups. The results of this study showed that the orientation of the fibers does not influence the strength of composite resins and the incorporation of nylon nanofibers with carbon nanotubes decreased the fracture resistance values. The presence of the fibers has not been able to improve the strength of the material in any of the...

Influência da incorporação de nanofibras de poliamida 6 com e sem nanotubos de carbono como reforço de prótese parcial fixa adesiva

The aim of this study was to evaluate the behavior of reinforced composites with polyamide 6 fibers aligned (6000 rpm) and alignment (120 rpm) with or without CNT using the flexural strength test. After preparation of nanofibers aligned nylon 6 (6000 rpm) and alignment (120 rpm) with and without incorporation of nanotube carbon by the method of electrospinning, were performed one control group (n = 10) and 4 experimental groups (n = 40) G1: Control (just resin Charisma - Heraeus Kulzer) ;G2 Resin + N6 aligned (6000 rpm) + CNT; G3:Resin + N6 alignment (120 rpm) + CNT; G4: Resin + aligned ( 6000 rpm) N6. G5: Resin + N6 alignment (120 rpm). The fibers were cut to the dimensions of 0,3 x 15 mm and were applied an adhesive at the surface (Single Bond 2) for 5 min and cured. In the matrix, was added resin in the proximal box (Charisma A2, Heraeus Kulzer) and cured for 40 s. (power 1100 mW / cm²). A first layer of resin and on the resin was deposited. The resin layers specimens were light irradiated with three overlapping exposures delivered. For each resin layer were light irradiated for 40 sec. The samples were tested with a cross-speed of 1 mm / min, and a 50 Kgf at Universal testing machine (EMIC mod.DL2000). The Dunnet test showed that only the nanotube group was significantly different from the control group. The ANOVA two-way indicates that the nanotube factor was statistically significant (p < 0.05) and there is no interaction between factors and orientation nanotube. The presence of nanotube showed lower fracture resistance values for aligned and unaligned groups. The results of this study showed that the orientation of the fibers does not influence the strength of composite resins and the incorporation of nylon nanofibers with carbon nanotubes decreased the fracture resistance values. The presence of the fibers has not been able to improve the strength of the material in any of the...

Graphene modification with gold nanoparticles using the gas aggregation technique

Gold nanoparticles (Au-NPs) were deposited on single layer graphene (SLG) and few layers graphene (FLG) by applying the gas aggregation technique, previously adapted to a 4-gun commercial magnetron sputtering system. The samples were supported on SiO2 (280 nm)/Si substrates, and the influence of the applied DC power and deposition times on the nanoparticle-graphene system was investigated by Confocal Raman Microscopy. Analysis of the G and 2D bands of the Raman spectra shows that the integrated intensity ratio (I-2D/I-G) was higher for SLG than for FLG. For the samples produced using a sputtering power of 30W, the intensity (peak height) of the G and 2D bands increased with the deposition time, whereas for those produced applying 60W the peak heights of the G and 2D bands decreased with the deposition time. This behaviour was ascribed to the formation of larger Au-NPs aggregates in the last case. A significant increase of the Full Width Half Maximum (FWHM) of the G band for SLG and FLG was also observed as a function of the DC power and deposition time. Surprisingly, the fine details of the Raman spectra revealed an unintentional doping of SLG and FLG accompanying the increase of size and aggregation of the Au-NPs. (C) 2011 Elsevier B.V. All rights reserved.

An Alternative Method for the Simultaneous Determination of Copper and Lead for Quality Control of Sugar Cane Spirit using a Nanotube-Based Sensor

The development of an electroanalytical method for simultaneous determination of copper and lead ions in sugar cane spirit (cachaca) using carbon paste electrode modified with ascorbic acid and carbon nanotubes (CPE-AaCNT) is described. Squarewave voltammetry (SWV) with anodic stripping was employed, and this technique was optimized with respect to the following parameters: frequency (50 Hz), amplitude (100 mV) and scan increment (9 mV). The analytical curves were linear in the range from 0.0900 to 7.00 mg L-1 for lead and copper. The limits of detection were 48.5 and 23.9 mu g L-1 for lead and copper, respectively. The developed method was applied to the simultaneous determination of copper and lead in five commercial samples of sugar cane spirit. The results were in good agreement with those obtained by F AAS/GF AAS (flame atomic absorption spectrometry/graphite furnace atomic absorption spectrometry) and showed that CPE-AaCNT can be successfully employed in the simultaneous determination of these metals in real sugar cane spirit samples.

Real-time electrochemical determination of phenolic compounds after benzene oxidation

A sensitive electrochemical sensor was successfully developed on multi-walled carbon nanotubes (MWCNT) and cobalt phthalocyanine (CoPc) modified glassy carbon electrode (GC), and used to detect byproducts formed after the electrolysis of benzene. The GC/MWCNT/CoPc electrode was applied in the detection of phenolic compounds using square wave voltammetry (SWV). The proposed sensor exhibited a sequence in the sensitivity of the tested phenols: catechol > hydroquinone > resorcinol > phenol and 1,4-benzoquinone. The detection limits for individual phenols were also calculated: catechol (15.62 mu g L-1), hydroquinone (17.91 mu g L-1), resorcinol (46.12 mu g L-1), phenol (58.83 mu g L-1) and 1,4-benzoquinone (13.75 mu g L-1). The proposed sensor was successfully applied in the determination of the total amount of phenols formed after the benzene oxidation, and the obtained results were in full agreement with those from the HPLC procedure. (C) 2012 Elsevier B.V. All rights reserved.

Nanoassisted Laser Desorption-Ionization-MS Imaging of Tumors

The ability of nanoassisted laser desorption-ionization mass spectrometry (NALDI-MS) imaging to provide selective chemical monitoring with proper spatial distribution of lipid profiles from tumor tissues after plate imprinting has been tested. NALDI-MS imaging identified and mapped several potential lipid biomarkers in a murine model of melanoma tumor (inoculation of B16/F10 cells). It also confirmed that the in vivo treatment of tumor bearing mice with synthetic supplement containing phosphoethanolamine (PHO-S) promoted an accentuated decrease in relative abundance of the tumor biomarkers. NALDI-MS imaging is a matrix-free LDI protocol based on the selective imprinting of lipids in the NALDI plate followed by the removal of the tissue. It therefore provides good quality and selective chemical images with preservation of spatial distribution and less interference from tissue material. The test case described herein illustrates the potential of chemically selective NALDI-MS imaging for biomarker discovery.

Enzymatic Solid-Phase Reactor Based on Silica Organofunctionalized with p-Phenylenediamine for Electrochemical Detection of Phenolic Compounds

A new biomaterial, based on silica organofunctionalized with p-phenylenediamine (p-PDA) and the enzyme peroxidase, was used in the development of an enzymatic solid-phase reactor. The analytical techniques used in the characterization showed that the organic ligand was incorporated into the silica matrix. Thus, the silica modified with p-PDA allowed the incorporation of peroxidase by the electrostatic interaction between the carboxylic groups present in the enzyme molecules and the amino groups attached to the silica. The enzymatic solid-phase reactor was used for chemical oxidation of phenols in 1, 4-benzoquinone that was then detected by chronoamperometry. The system allowed the analysis of hydroquinone with a detection limit of 83.6 nmol L-1. Thus, the new material has potential in the determination of phenolic compounds river water samples.

Platinum nanoparticles incorporated in silsesquioxane for use in LbL films for the simultaneous detection of dopamine and ascorbic acid

We describe the preparation of platinum nanoparticles (PtNPs) using the 3-n-propylpyridinium silsesquioxane chloride (SiPy+Cl-) as a nanoreactor and stabilizer. The formation of PtNPs was monitored by UV-Vis spectroscopy by measuring the decrease in the intensity of the band at 375 nm, which is attributed to the electronic absorption of PtCl62- ions. TEM images of Pt-SiPy+Cl- nanohybrid indicated an average size of 3-40 nm for PtNPs. The Pt-SiPy+Cl- was used as a polycation in the preparation of layer-by-layer films (LbL) on a glass substrate coated with fluorine-doped tin oxide (FTO) alternating with the polyanion poly(vinyl sulfonic acid) (PVS). The films were electrochemically tested in sulfuric acid to confirm the deposition of Pt-SiPy+Cl- onto the LbL films, observing the adsorption and desorption of hydrogen (E-pa = 0.1 V) and by the redox process of formation for PtO with E-pa = 1.3 V and E-pc = 0.65 V. FTIR and Raman spectra confirmed the presence of the PVS and Pt-SiPy+Cl- in the LbL films. A linear increase in the absorbance in the UV-Vis spectra of the Pt-SiPy+Cl- at 258 nm (pi -> pi* transition of the pyridine groups) with a number of Pt-SiPy+Cl-/PVS or PVS/SiPy+Cl- bilayers (R = 0.992) was observed. These LbL films were tested for the determination of dopamine (DA) in the presence of ascorbic acid (AA) with a detection limit (DL) on the order of 2.6 x 10(-6) mol L-1 and a quantification limit (QL) of 8.6 x 10(-6) mol L-1. The films exhibited a good repeatability and reproducibility, providing a potential difference of 550 mV for the oxidation of DA with AA interferent.