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1.
ChemSusChem ; : e202301671, 2024 May 10.
Artigo em Inglês | MEDLINE | ID: mdl-38728171

RESUMO

Carbon materials are readily available and are essential in energy storage. One of the routes used to enhance their surface area and activity is the decoration of carbons with semiconductors, such as amorphous TiO2, for application in energy storage devices. This work reports the preparation of amorphous TiO2 nanopowders, which were obtained through the anodization of titanium in ethaline media. The obtained amorphous TiO2 was used to obtain TiO2-decorated carbon (obtained through the carbonization of glycogen precursor from mussel cooking wastewater, under N2 atmosphere) composites through three different methods: electrochemical in-situ attachment of TiO2 nanopowders to the carbon matrix using ultrasounds and sonication in ethaline. Commercial TiO2 was used as the comparison material. Morphology, composition, and structure analysis were performed, followed by the electrochemical analysis in ethaline electrolyte. The in-situ attachment of amorphous TiO2 to the carbon matrix shows the most promising electrochemical performance of 956 F g-1 at 1 A g-1 for the three-electrode cell setup, with 100%  and 98% capacitance retention after 1000 and 10000 cycles. On a two-electrode symmetric solid-state electrolyte cell, the gravimetric capacitance is 1251 F g-1, at 1 A g-1, with 90% and 78% capacitance retention after 1000 and 10000 cycles, respectively.

2.
Langmuir ; 40(15): 7947-7961, 2024 Apr 16.
Artigo em Inglês | MEDLINE | ID: mdl-38578030

RESUMO

This work presents the synthesis of CoSb3 one-dimensional (1D) thermoelectric nanomaterials using electrodeposition under galvanostatic conditions and polycarbonate membranes as a template (50 nm diameter pores). Cyclic voltammetry measurements have been performed to get preliminary information on the electrochemical reduction process of the involved species. Different current density values in the range 1-4 mA cm-2 have been applied, leading to the formation of nanowires (NWs) and micro- and nanomushroom caps, as evidenced by the scanning electron microscopy and scanning transmission electron microscopy investigations. Through fine-tuning of the current density the desired Co/Sb atomic ratio could be achieved. Energy-dispersive X-ray spectroscopy analysis showed the formation of CoSb3 at 1.4 mA cm-2, and it has also been confirmed by high-resolution transmission electron microscopy and micro-Raman spectroscopy. In this work, we present for the first time the fabrication of a CoSb3-CoxSby heterojunction on the same NW exhibiting Sb-rich and Co-rich alloy segments, prepared by electrodeposition from the same electrolyte by simply varying the applied current density.

3.
Nanomaterials (Basel) ; 12(21)2022 Oct 27.
Artigo em Inglês | MEDLINE | ID: mdl-36364561

RESUMO

Porous InP templates possessing a thickness of up to 100 µm and uniformly distributed porosity were prepared by anodic etching of InP substrates exhibiting different electrical conductivities, involving an environmentally friendly electrolyte. Ni nanoparticles were successfully directly deposited by pulsed electroplating into prefabricated InP templates without any additional deposition of intermediary layers. The parameters of electrodeposition, including the pulse amplitude, pulse width and interval between pulses, were optimized to reach a uniform metal deposition covering the inner surface of the nanopores. The electrochemical dissolution of n-InP single crystals was investigated by measuring the current-voltage dependences, while the Ni-decorated n-InP templates have been characterized by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The proposed technology is expected to be of interest for sensing and photocatalytic applications, as well as for the exploration of their plasmonic and magnetic properties.

4.
Nanomaterials (Basel) ; 12(16)2022 Aug 14.
Artigo em Inglês | MEDLINE | ID: mdl-36014653

RESUMO

A high-luminescent, blue-light excitable europium(III) coordination complex, [Eu(µ2-OC2H5)(btfa)(NO3)(phen)]2phen (1) {btfa = benzoyl trifluoroacetone, phen = 1,10-phenantroline}, has been synthesized and investigated. The complex was characterized by infrared (IR) and photoluminescence (PL) spectroscopy. The PL emission spectra of powder samples registered in a range of 10.7-300 K exhibit characteristic metal-centered luminescence bands, assigned to internal radiative transitions of the Eu3+ ion, 5D1→7Fj and 5D0→7Fj (j = 0-4). The high-resolution spectrum of the transition 5D0→7F0 shows that it consists of two narrow components, separated by 0.96 meV, which indicates the presence in the matrix of two different sites of the Eu3+ ion. The splitting pattern of 5D0→7Fj (j = 0-4) transitions indicates that europium ions are located in a low-symmetry environment. The absolute quantum yield and the sensitization efficiency were determined to be 49.2% and 89.3%, respectively. The complex can be excited with low-cost lasers at around 405 nm and is attractive for potential applications in optoelectronics and biochemistry.

5.
Nanomaterials (Basel) ; 12(3)2022 Jan 22.
Artigo em Inglês | MEDLINE | ID: mdl-35159693

RESUMO

Our work presents, for the first time, a comprehensive study of the synthesis of fully metallic platinum nanoparticles (Pt-NPs) involving the ablation process in double distilled water using a KrF excimer laser. To obtain detailed information on Pt-NP morphology and optical properties, prepared colloids were characterized using High Resolution Scanning Transmission Electron Microscopy (HR-STEM) with advanced capabilities for Energy Dispersive X-ray Analysis (EDX), UV/Vis optical spectroscopy, and Direct Analysis in Real Time-Mass Spectrometry (DART-MS). The influence of the applied laser fluence and laser repetition rate (RR) values on the characteristics of the obtained Pt-NPs and the ablation process, respectively, were also analyzed. Spherical and spherical-like nanoparticles exhibiting aggregation were produced. The Pt-NP mean size values were between 2.2 ± 1.2 nm and 4.0 ± 1.0 nm, while their interplanar distance measurements showed a face-centered cubic (FFC) Pt lattice (111), as revealed by HR-STEM measurements, for all investigated samples. The smallest mean size of 2.2 nm of the Pt-NPs was obtained using a 2.3 J cm-2 laser fluence at a 10 Hz RR, and the narrowest size distribution of the NPs was obtained with a 2.3 J cm-2 laser fluence at a 40 Hz RR. A linear dependence of the Pt-NP diameters versus the laser repetition rate was found at a constant fluence of 2.3 J cm-2. The proposed eco-friendly synthesis route of Pt-NPs, because of its relative simplicity, has the potential for use in industrial production.

6.
Polymers (Basel) ; 13(7)2021 Apr 02.
Artigo em Inglês | MEDLINE | ID: mdl-33918350

RESUMO

Single wall carbon nanotubes (SWCNTs) were grown on either sized or desized carbon fabric in a self-designed reactor by Pulsed Laser Deposition (PLD). The uniqueness of the PLD system lies, among other things, in the ability to keep the substrate at a low temperature, compared to the 1100 °C needed for the SWCNTs synthesis, thus, rendering it undamaged. Samples were placed at different positions on a cold finger (CF), where a temperature gradient develops, in the range 25-565 °C. The chemical composition and morphology of desized and surface treatments, as well as SWCNTs grown on carbon fibres, were verified by Scanning Electron Microscopy (SEM) equipped with Energy Dispersive X-Ray Spectroscopy (EDX), while the quality of SWCNTs was proven by confocal micro-Raman Spectroscopy and High-Resolution Scanning Transmission Electron Microscopy (HR-STEM). Fibres covered with SWCNTs by PLD were characterized using contact angle and the surface free energy was calculated. A micro-droplet pull-out test was used to evaluate the effect of SWCNTs over interfacial properties of a carbon-epoxy composite. A 20% increase in interfacial shear strength (IFSS) was observed by deposition at 290 °C, compared to the commercial carbon fibre sizing. The carbon fibres kept their tensile properties due to the low deposition temperatures.

7.
J Mech Behav Biomed Mater ; 112: 104084, 2020 12.
Artigo em Inglês | MEDLINE | ID: mdl-32949866

RESUMO

The present work introduces nanostructured Zr as a possible choice of metallic implant biomaterial in competition with titanium and its new alloys. The paper reports on the preparation of anodized zirconium in a mixture of electrolytes with fluoride ions, 1 M (NH4)2SO4 + 0.15 M NH4F + distilled water, at 20 V. The obtained nanostructures were investigated by SEM, EDX, XRD and AFM techniques. The SEM - EDX longitudinal and cross sectional analysis revealed the morphology of the formed oxide layers and their thicknesses, which were found to be 7.45 ± 0.18 µm. The mean nanopores' diameter was calculated as 15.8 ± 3.3 nm. The XRD investigations enabled the evaluation of crystallite sizes and texture coefficients for zirconium and zirconium oxide containing samples. The inhibition effect against Escherichia coli and Streptococcus Aureus bacteria was evaluated and discussed as well. The AFM studies revealed that the nano-porous Zr has similar hardness parameter as the uncoated Zr, but lower surface adhesion force that could be translated into improved properties in terms of antimicrobial effects, as confirmed by its inhibition index, which makes it a very promising material for bio-medical applications.


Assuntos
Fluoretos , Zircônio , Estudos Transversais , Microscopia Eletrônica de Varredura , Propriedades de Superfície , Titânio
8.
ACS Appl Mater Interfaces ; 11(11): 10785-10793, 2019 Mar 20.
Artigo em Inglês | MEDLINE | ID: mdl-30788961

RESUMO

Push-coating is a simple process that can be employed for extremely low-cost polymer electronic device production. Here, we demonstrate its application to the fabrication of poly(2,7-carbazole- alt-dithienylbenzothiadiazole) (PCDTBT):[6,6]-phenyl-C71-butyric acid methyl ester (PC71BM) active layers processed in air, yielding similar photovoltaic performances as thermally annealed spin-coated thin films when used in inverted polymer solar cells (PSCs). During push-coating, the polydimethylsiloxane layer temporarily traps the deposition solvent, resulting in simultaneous film formation and solvent annealing effect. This removes the necessity for a postdeposition thermal annealing step which is required for spin-coated PSCs to produce high photovoltaic performances. Optimized PSC active layers are produced with a push-coating time of 5 min at room temperature with 20 times less hazardous solvent and 40 times less active material than spin-coating. Annealed spin-coated active layers and active layers push-coated for 5 min both produce average power conversion efficiencies (PCEs) of 5.77%, while those push-coated for a shorter time of 1 min yield a slightly lower value of 5.59%. We demonstrate that, despite differences in their donor:acceptor vertical concentration gradients, unencapsulated PCDTBT:PC71BM active layers push-coated for 1 min produce PSCs with similar operational stability and upscaling capacity as thermally annealed spin-coated ones. As fast device fabrication can be achieved with short-time push-coating, we further demonstrate the potential of this deposition technique by manufacturing push-coated PSC-based semitransparent photovoltaic devices with a PCE of 4.23%, relatively neutral colors and an average visible transparency of 40.2%. Our work thus confirms that push-coating is not limited to the widely employed poly(3-hexylthiophene-2,5-diyl) but can also be used with low band gap copolymers and opens the path to low-cost and eco-friendly, yet efficient and stable PSCs.

9.
Pharmaceutics ; 10(4)2018 Nov 09.
Artigo em Inglês | MEDLINE | ID: mdl-30423969

RESUMO

The aim of this study is to design, develop and evaluate new biohybrid sponges based on polymers (collagen and polyvinyl alcohol) with and without indomethacin as anti-inflammatory drug model to be used for tissue regeneration in wound healing. Type I fibrillar collagen in the form of a gel and different concentrations of polyvinyl alcohol were mixed together to prepare composite gels. Both control samples, without indomethacin and with indomethacin, were obtained. All samples were crosslinked with glutaraldehyde. By freeze-drying of hydrogels, the spongious forms (matrices) were obtained. The matrices were characterized by FT-IR spectroscopy, scanning electron microscopy (SEM), water absorption, enzymatic degradation and in vitro indomethacin release. The pharmacological effect of the spongious biohybrid matrices was determined on an experimental model of burns induced to Wistar rats. The SEM images showed a porous structure with interconnected pores. Collagen sponges present a structure with pore sizes between 20 and 200 µm, which became more and more compact with polyvinyl alcohol addition. The FT-IR showed interactions between collagen and polyvinyl alcohol. The enzymatic degradation indicated that the most stable matrix is the one with the ratio 75:25 of collagen:polyvinyl alcohol (ACI75), the other ones being degradable in time. The kinetic data of indomethacin release from matrices were fitted with different kinetic models and highlighted a biphasic release of the drug. Such kinetic profiles are targeted in skin wound healing for which important aspects are impaired inflammation and local pain. The treatment with sponges associated with anti-inflammatory drug had beneficial effects on the healing process in experimentally induced burns compared to the corresponding matrices without indomethacin and the classical treated control group.

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