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1.
Chem Commun (Camb) ; 56(5): 802-805, 2020 Jan 16.
Artigo em Inglês | MEDLINE | ID: mdl-31848555

RESUMO

We present the unprecedented application of a black phosphorus-based nanocomposite as an electrode for aqueous Na-ion batteries under ambient conditions. An impressive specific capacity of up to 200 mA h g-1 was reached after 50 cycles in a NaCl aqueous solution used as a supporting electrolyte. Post-characterization indicated the integrity of the black phosphorus.

2.
J Colloid Interface Sci ; 554: 80-90, 2019 Oct 15.
Artigo em Inglês | MEDLINE | ID: mdl-31279276

RESUMO

We report a simple and effective route to synthesize, disperse, exfoliate and process different molybdenum-based 2-dimensional (2D) materials. Starting from a reaction between ammonium molybdate and ammonium sulfide solutions, a powder consisting of a mixture between amorphous molybdenum oxide and sulfide is obtained. By tuning the atmosphere and the temperature, different compositions can be prepared by thermal treatment of this sample: heat treatments in ambient atmosphere produce MoO3 with different morphologies, controllable according to the chosen temperature. On the other hand, heat treatments in inert atmosphere produce mixtures between crystalline 2D MoS2 and MoO3. Further handling of these mixtures with acetonitrile separates the components due to the different solvent/solid affinities, with the layered MoS2 becoming homogeneously dispersed, and the MoO3 agglomerating as a solid easily removed by centrifugation. The resulting sulfide dispersions in acetonitrile present high stability, and they are constituted by exfoliated MoS2, which means that acetonitrile is a tri-functional agent, separating the sulfide/oxide mixture, exfoliating the sulfide and stabilizing the dispersion. The MoS2 dispersions were used to produce homogeneous, freestanding and transparent thin films through the liquid-liquid interfacial route, which were easily deposited over different substrates and characterized by different techniques.

3.
Chem Commun (Camb) ; 55(41): 5809-5812, 2019 May 16.
Artigo em Inglês | MEDLINE | ID: mdl-31041936

RESUMO

A novel methodology to prepare stable aqueous dispersions of raw single- and multi-walled carbon nanotubes is reported, based on dispersions previously prepared in tetrahydrofuran containing a phenol that donates electrons to nanotubes and provides colloidal stability through electrostatic repulsion. A proposed mechanism for the stabilization of the dispersions is presented. Conductive and transparent thin films are prepared through a liquid/liquid interfacial route starting from these dispersions.

4.
Phys Chem Chem Phys ; 21(2): 736-743, 2019 Jan 02.
Artigo em Inglês | MEDLINE | ID: mdl-30543327

RESUMO

The conducting polymer, poly(3,4-ethylenedioxythiophene)-polystyrenesulfonic acid (PEDOT:PSS), is certainly one of the most important substitute materials for indium tin oxide in organic devices. Its metallic conductivity and transmittance bring favorable perspectives for organic photovoltaic applications. Although graphene oxide (GO) is not a good conductor, it can form high-quality thin films and can be transparent, and additionally, GO is an inexpensive material and can be easily synthesized. This study investigated how the conductivity of a composite film of graphene oxide (GO) and different amounts of PEDOT:PSS can be modified. The effects of GO:PEDOT:PSS composites with several PEDOT:PSS proportions were analyzed in regards to the composite molecular structure and ordering, charge transfer dynamics (in the femtosecond range), electrical properties and morphology. For the best conductivity ratio GO found with 5% PEDOT:PSS, a solvent treatment was also performed, comparing the resistivity of the film when treated with dimethyl sulfoxide (DMSO) and with ethylene glycol.

5.
Chem Sci ; 9(37): 7297-7303, 2018 Oct 07.
Artigo em Inglês | MEDLINE | ID: mdl-30294418

RESUMO

The largest graphene sample obtained through a chemical reaction under ambient conditions (temperature and pressure), using simple molecules such as benzene or n-hexane as precursors, is reported. Starting from a heterogeneous reaction between solid iron chloride and the molecular precursor (benzene and n-hexane) at a water/oil interface, graphene sheets with micrometric lateral size are obtained as a film deposited at the liquid/liquid (L/L) interface. The pathway involving the cyclization and aromatization of n-hexane to benzene at the L/L interface, and the sequence of conversion of benzene to biphenyl and biphenyl to condensed rings (which originates the graphene structures) was followed by different characterization techniques and a mechanistic proposal is presented. Finally, we demonstrate that this route can be extended for the synthesis of N-doped graphene, using pyridine as the molecular precursor.

6.
J Colloid Interface Sci ; 529: 187-196, 2018 Nov 01.
Artigo em Inglês | MEDLINE | ID: mdl-29894937

RESUMO

Dispersing carbon nanotubes is an easy and low-cost way to manipulate these solids and allows the preparation of more complex materials or devices, so it is fundamental for further uses that these dispersions have controlled properties and high colloidal stability. In this work we report the spontaneous electrical charge build-up in pristine multi-walled carbon nanotubes dispersed in common organic solvents such as chloroform and tetrahydrofuran and the achievement of dispersions stable for long periods without adding passivant agents or functional groups on nanotubes surface. Results from electrokinetics, homo- and heterocoagulation provided macroscopic evidences that carbon nanotubes acquire electric charges after dispersion in some organic liquids and we confirmed this process by measuring in situ Raman spectra of the nanotubes dispersions with higher surface electric potentials. We also show that the signal of electric potential of the dispersions can be predicted by the acid-base behaviour of the dispersing medium, corroborating previously reports for other dispersions of carbon nanomaterials.

7.
Biosens Bioelectron ; 112: 108-113, 2018 Jul 30.
Artigo em Inglês | MEDLINE | ID: mdl-29702381

RESUMO

The modification of electrode surfaces has been the target of study for many researchers in order to improve the analytical performance of electrochemical sensors. Herein, the use of an imidazole-functionalized graphene oxide (GO-IMZ) as an artificial enzymatic active site for voltammetric determination of progesterone (P4) is described for the first time. The morphology and electrochemical performance of electrode modified with GO-IMZ were characterized by scanning electron microscopy and cyclic voltammetry, respectively. Under optimized conditions, the proposed sensor showed a synergistic effect of the GO sheets and the imidazole groups anchored on its backbone, which promoted a significant enhancement on electrochemical reduction of P4. Figures of merits such as linear dynamic response for P4 concentration ranging from 0.22 to 14.0 µmol L-1, limit of detection of 68 nmol L-1 and limit of quantification and 210 nmol L-1 were found. In addition, presented a higher sensitivity, 426 nA L µmol-1, when compared to the unmodified electrode. Overall, the proposed device showed to be a promising platform for a simple, rapid, and direct analysis of progesterone.


Assuntos
Técnicas Biossensoriais , Técnicas Eletroquímicas , Progesterona/isolamento & purificação , Grafite/química , Humanos , Imidazóis , Limite de Detecção , Microscopia Eletrônica de Varredura , Óxidos/química , Progesterona/química
8.
ChemSusChem ; 11(7): 1238-1245, 2018 04 09.
Artigo em Inglês | MEDLINE | ID: mdl-29438585

RESUMO

Most of the dye-sensitized solar cells (DSSCs) developed so far use organic electrolytes and water-sensible sensitizers. The search for aqueous DSSCs, a promising technology for solar-energy conversion, implies finding materials that are stable in aqueous solution. In this study, Prussian blue (PB) was utilized as an innovative sensitizer in a photoanode for DSSCs and a novel synthetic approach to a carbon nanotubes/TiO2 /PB nanocomposite thin film was developed. The photoresponse was evaluated in a total aqueous electrolyte, and photocurrents of 600 µA cm-2 were achieved.

9.
ACS Omega ; 3(2): 1367-1373, 2018 Feb 28.
Artigo em Inglês | MEDLINE | ID: mdl-31458465

RESUMO

Environmentally friendly multifunctional rubber composites are reported. Graphitic nanocarbon (NC) deriving from cracking of biogas (methane/carbon dioxide) and natural rubber extracted directly from the Hevea brasiliensis tree are the two components of these composites produced via latex technology. While maintaining and enhancing the intrinsic thermal and mechanical characteristics of rubber, the presence of NC shows a significant improvement on the electrical response. For a 10 wt % NC content, a 1010-fold increase in conductivity has been achieved with a conductivity value of 7.5 S·m-1, placing these composites among the best obtained using other carbon fillers. In addition, the piezoresistive behavior has also been verified. These promising green composites have a potential use in a variety of applications such as sealing of electronic devices and sensors.

10.
Sci Rep ; 7(1): 10165, 2017 08 31.
Artigo em Inglês | MEDLINE | ID: mdl-28860636

RESUMO

The greatest challenge regarding black phosphorus (BP) comes as a result of its fast degradation when exposed to ambient conditions, which has overshadowed its applications. Herein, we report a simple and efficient route towards overcoming BP deterioration by preparing a nanocomposite with the conducting polymer polyaniline (PANI). The liquid/liquid interfacial method was employed to produce transparent, freestanding and transferable thin film of BP covered by PANI, with high stability under ambient atmosphere, up to 60 days. Otherwise, the uncapped exfoliated neat BP degraded in solely 3 days under the same conditions. Characterization data show that PANI covers efficiently the BP flakes, indicating favorable interactions between the components. The results presented here can be considered a breakthrough for employing BP as thin film in different technological applications, considering the properties of BP itself or taking advantage of synergistically combining the properties of both components.

11.
Mater Sci Eng C Mater Biol Appl ; 79: 262-269, 2017 Oct 01.
Artigo em Inglês | MEDLINE | ID: mdl-28629017

RESUMO

This study describes a new route for preparation of a nanocomposite between graphene oxide (GO) and bismuth nanoparticles (BiNPs) and its evaluation as modifier electrode for development of electrochemical sensors. BiNPs were synthesized under ultrasound conditions using Bi(NO3)3 as metal precursor and ascorbic acid (AA) as reducing agent/passivating. Some experimental parameters of BiNPs synthesis such as Bi3+:AA molar ratio and reaction time were conducted aiming the best voltammetric performance of the sensor. Glassy carbon electrodes (GCE) were modified by drop-casting with the BiNPs dispersions and anodic stripping voltammetry measurements were performed and revealed an improvement in the sensitivityfor determination of Cd(II) and Pb(II) compared to an unmodified electrode. The best electrochemical response was obtained for a BiNPs synthesis with Bi3+:AA molar ratio of 1:6 and reaction time of 10min, which yielded Bi metallic nanoparticles with average size of 5.4nm confirmed by XRD and TEM images, respectively. GO was produced by graphite oxidation using potassium permanganate and exfoliated with an ultrasound tip. GO-BiNPs nanocomposite was obtained by a simple mixture of GO and BiNPs dispersions in water and kept under ultrasonic bath for 1h. GCE were modified with a nanocomposite suspension containing 0.3 and 1.5mgmL-1 of GO and BiNPs in water, respectively. Under optimized conditions, the proposed nanocomposite was evaluated on the voltammetric determination of Pb (II) and Cd (II), leading to a linear response range between 0.1 and 1.4µmolL-1 for both cations, with limit of detection of 30 and 27nmolL-1, respectively. These results indicate the great potential of the GO-BiNPs nanocomposite for improving the sensitivity of voltammetric procedures.


Assuntos
Nanopartículas Metálicas , Bismuto , Técnicas Eletroquímicas , Eletrodos , Grafite , Óxidos
12.
J Colloid Interface Sci ; 502: 146-152, 2017 Sep 15.
Artigo em Inglês | MEDLINE | ID: mdl-28478221

RESUMO

Conducting and transparent interfacial thin films have been prepared from double-walled carbon nanotubes (DWCNT) and further deposited over glass and plastic (polyethylene terephtalate-PET) substrates. The morphology, vibrational structure as well as the optical and electrical properties have been evaluated. The influence of the DWCNT purifying treatment, the amount of carbon nanotubes used to prepare the thin films, and the annealing of the films at different temperatures has been evaluated to optimize both electrical and optical properties. Values of sheet resistance ranging from 0.53 to 27.8 kΩ â–¡-1 and transmittance at 550nm from 59 to 90% have been achieved. Similar behavior obtained for films deposited on PET or glass substrates indicate a good reproducibility of the method, besides the high potential for further applications on flexible devices.

13.
Sci Rep ; 6: 33806, 2016 Sep 22.
Artigo em Inglês | MEDLINE | ID: mdl-27654065

RESUMO

Different nanocomposites between reduced graphene oxide (rGO) and Ni(OH)2 nanoparticles were synthesized through modifications in the polyol method (starting from graphene oxide (GO) dispersion in ethylene glycol and nickel acetate), processed as thin films through the liquid-liquid interfacial route, homogeneously deposited over transparent electrodes and spectroscopically, microscopically and electrochemically characterized. The thin and transparent nanocomposite films (112 to 513 nm thickness, 62.6 to 19.9% transmittance at 550 nm) consist of α-Ni(OH)2 nanoparticles (mean diameter of 4.9 nm) homogeneously decorating the rGO sheets. As a control sample, neat Ni(OH)2 was prepared in the same way, consisting of porous nanoparticles with diameter ranging from 30 to 80 nm. The nanocomposite thin films present multifunctionality and they were applied as electrodes to alkaline batteries, as electrochromic material and as active component to electrochemical sensor to glycerol. In all the cases the nanocomposite films presented better performances when compared to the neat Ni(OH)2 nanoparticles, showing energy and power of 43.7 W h kg-1 and 4.8 kW kg-1 (8.24 A g-1) respectively, electrochromic efficiency reaching 70 cm2 C-1 and limit of detection as low as 15.4 ± 1.2 µmol L-1.

14.
J Colloid Interface Sci ; 478: 107-16, 2016 Sep 15.
Artigo em Inglês | MEDLINE | ID: mdl-27288576

RESUMO

Thin films of either unpurified single-walled carbon nanotubes (SWCNT) or iron-filled multi-walled carbon nanotubes (MWCNT) were deposited through the liquid-liquid interfacial route over plastic substrates, yielding transparent, flexible and ITO-free electrodes. The iron species presented in both electrodes (inside of the MWCNT cavities or outside of the SWCNT bundles, related to the catalyst remaining of the growth process) were employed as reactant to the electrosynthesis of Prussian blue (PB), yielding carbon nanotubes/Prussian blue nanocomposite thin films, which were characterized by Raman spectroscopy, scanning electron microscopy, atomic force microscopy, cyclic voltammetry and galvanostatic charge/discharge measurements. The nanocomposite films were employed as cathodes for flexible, transparent and ITO-free potassium batteries, showing reversible charge/discharge behavior and specific capacitance of 8.3mAhcm(-3) and 2.7mAhcm(-3) for SWCNT/PB and MWCNT/PB, respectively.

15.
Chemistry ; 22(19): 6643-53, 2016 May 04.
Artigo em Inglês | MEDLINE | ID: mdl-27010671

RESUMO

Multi-walled carbon nanotubes (MWCNTs) filled with different species of cobalt (metallic cobalt, cobalt oxide) were synthesized by a chemical vapor deposition method through cobaltocene pyrolysis. A systematic study was performed to correlate different experimental conditions with the structure and characteristics of the obtained material. Thin films of Co-filled CNTs were deposited over conductive substrates through a liquid-liquid interfacial method and were used for cobalt hexacyanoferrate (CoHCFe) electrodeposition by an innovative route in which the Co species encapsulated in the CNTs were employed as reactants. The CNT/CoHCFe films were characterized by different spectroscopic, microscopic, and electrochemical techniques and presented high electrochemical stability in different media. The nanocomposites were applied as both an electrochemical sensor to H2 O2 and a cathode for ion batteries and showed limits of detection at approximately 3.7 nmol L(-1) and a capacity of 130 mAh g(-1) at a current density of 5 A g(-1) .

16.
J Colloid Interface Sci ; 467: 239-244, 2016 Apr 01.
Artigo em Inglês | MEDLINE | ID: mdl-26803603

RESUMO

We report a novel pKa determination for different graphene-like samples: graphene oxide (GO), reduced GO (rGO), graphene nanoribbons (GNR), oxidized GNR (GONR), thiol- and imidazole-functionalized GO (GOSH and GOIMZ, respectively) and thiol-functionalized GONR (GONRSH). Using the specialized computational program BEST7 for treating titration curves, pKas for different functional groups were discriminated (confirmed by infrared spectra) and their composition quantified. Overall, three equilibria were distinguished, two relative to carboxylic acids exhibiting different acidic degrees (pKa1∼4.0 and pKa2∼6.0) and one relative to alcohols (pKa4∼10.0). Upon functionalization on carboxylate sites, thiol (pKa(GOSH/GONRSH)=6.7) and imidazole (pKa(GOIMZ)=6.6) moieties were discerned, followed by a decrease of their carboxylate percentage (compared to the precursors), thus allowing determining the degree of functionalization (48% and 36% of thiol content for GOSH and GONRSH respectively, and 29% of imidazole for GOIMZ). The proposed method is innovative and simpler when compared to the traditional tools usually employed to quantify chemical functionalization.

17.
J Colloid Interface Sci ; 468: 34-41, 2016 Apr 15.
Artigo em Inglês | MEDLINE | ID: mdl-26821149

RESUMO

Hexagonal close packed (hcp) nickel nanoparticles stabilized by polyvinylpyrrolidone (PVP) were synthesized through the thermal treatment of face centered cubic (fcc) nickel nanoparticles. Controlling both the temperature of the heat treatment and the amount of PVP was possible the control of the hcp/fcc rate in the samples, where the higher Ni/PVP ratio produces only the hcp-nickel phase (average size of 8.9 nm) highly stable in air. The crystalline structure, the presence of PVP, the size of the nanoparticles and the stability of the hcp-nickel were confirmed using X-ray diffractometry, Fourier transform infrared spectroscopy, transmission electron microscopy, Raman spectroscopy, scanning electron microscopy and thermogravimetric analysis. Thin films of hcp and fcc nickel nanoparticles were prepared through a biphasic system and deposited over indium-doped tin oxide (ITO) substrates, which were electrochemically characterized and applied as glycerol amperometric sensors in NaOH medium. Parameters as the number of cycles applied and the scan rate were evaluated and indicate that hcp nickel nanoparticles are more reactive to form Ni(OH)2 and lead to more electroactive Ni(OH)2 structure. The hcp nickel nanoparticles-modified electrode showed the best sensitivity (0.258 µA L µmol(-1)) and detection limit (2.4 µmol L(-1)) toward glycerol.

18.
Chem Commun (Camb) ; 52(8): 1629-32, 2016 Jan 28.
Artigo em Inglês | MEDLINE | ID: mdl-26658554

RESUMO

A versatile and room temperature synthesis of thin films of polymer/graphene is reported. Drastically differing from other methods, not only the polymer but also the graphene are completely built from their simplest monomers (thiophene and benzene) in a one-pot polymerization reaction at a liquid-liquid interface. The materials were characterized and electronic properties are presented.

19.
J Colloid Interface Sci ; 453: 28-35, 2015 Sep 01.
Artigo em Inglês | MEDLINE | ID: mdl-25965429

RESUMO

Nanocomposites between nickel nanoparticles and graphene were obtained starting from nickel cations and graphenide solutions (negatively charged graphene layers) as both reducing agent to nickel cations and graphene source. Different nanomaterials were obtained in two different solvents, N-methyl-2-pyrrolidone (NMP) and tetrahydrofuran (THF), with different nickel/graphene ratios. The nanomaterials were characterized by UV-Vis spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray spectroscopy (EDS), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). All the samples consist of large graphene layers highly decorated with crystalline nickel nanoparticles, of size ranging from 2 to 10 nm. Thin films of the samples were deposited on indium-tin oxide (ITO) substrates and electrochemically characterized in alkaline medium, leading to Ni(OH)2/NiOOH redox pair, where the increase of the nickel proportion in the nanocomposites resulted in higher peak currents. The samples obtained in NMP showed the best performance with a fivefold increase of the peak currents, consistent with the lower charge transfer resistance as seen by electrochemical impedance spectroscopy (EIS).

20.
Dalton Trans ; 44(13): 5985-95, 2015 Apr 07.
Artigo em Inglês | MEDLINE | ID: mdl-25407673

RESUMO

This work reports the preparation, characterization and application as both electrochromic materials and electrochemical sensors of novel materials: carbon nanotubes/ruthenium purple nanocomposites. Using an innovative route based on a heterogeneous electrochemical reaction involving iron oxide species encapsulated within the cavities of the carbon nanotubes, the nanocomposite materials were obtained as transparent thin films deposited over transparent electrodes. Several experimental parameters related to the nanocomposite synthesis were evaluated and related to the characteristics of the obtained materials, such as morphology and stability. The films were characterized by UV-Vis and Raman spectroscopy, scanning electron microscopy, X-ray diffraction, cyclic voltammetry and UV-Vis and Raman spectroelectrochemistry. Four different materials were applied as H2O2 sensors and exhibited impressive analytical parameters, including a limit of detection of 1.27 nmol L(-1) and a sensitivity of 39.6 A M(-1) cm(-2). These nanocomposites also showed great electrochromic properties, with high stability and coloration efficiency over 95% maintained during stability cycles.

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