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In the present work, attempts of reducing a graphene oxide powder using a low temperature hydrogenation disproportionation desorption and the recombination process (L-HDDR) has been carried out. A lower processing temperature in large scale production is significant when costs are concerned. Graphite oxide was prepared using a modified Hummers’ method dispersed in ethanol and exfoliated using ultrasonication to produce Graphene Oxide (GO). Investigations have been carried out by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The experimental results of L-HDDR processing graphene oxide powder, using unmixed hydrogen at 400°C and relatively low pressures (

In this article the results of the negative electrode performance produced by La0.7Mg0.3Al0.3Mn0.4Co0.5Ni3.8 as-cast alloy adding 1 to 10% of carbon nanotube (CNT) or reduced graphene oxide (rGO) were investigated as Ni-MH batteries. The as cast alloy were investigated with X-ray diffraction (XRD) and scanning electron microscopy (SEM). The CNT and rGO were characterized by high resolution SEM-FEG. The discharge capacity obtained during the electrochemical characterization showed that in the addition of 1% rGO the discharge capacity was 332 mAh and 1% CNT 364 mAh , being that the rGO batteries maintaining better cyclic stability during the electrochemical test.

The equivalent series resistances (ESR) and specific capacitances (Cs) of supercapacitors carbon electrodes have been investigated using cyclic voltammetry and electrochemical impedance spectroscopy. Commercial activated carbon electrodes employing organic electrolyte have been tested using a potential window in the range of 2.7–3.8 V. Specific capacitances were calculated from cyclic voltammetry curves at room temperature employing various scan rates (30 and 100mVs-1). Internal series resistances of the supercapacitors were measured using the galvanostatic curves at room temperature and above (25 and 50°C). The ESR increase to 9.8 Ω at 25° and 2.7V to 78.8 Ω at with operating temperature raise and also with overpotential. A compositional and morphological evaluation of these electrodes showed a very homogeneous structure. It has been shown that the specific capacitance decreased considerably with scan rate, current density, electrochemical potential window and working temperature.

The effects of the separator thickness (δ) upon the equivalent series resistances (ESR) and specific capacitances (Cs) of supercapacitors electrodes have been investigated using commercially available porous filter paper (δ=150 μm, pores size=7.5 μm, 80 gm-2). Commercial activated carbon electrodes immersed in 1molL-1 KOH electrolyte (25°C) have been employed in this study. The specific capacitances were calculated from cyclic voltammetry curves at room temperature employing various scan rates (5, 10, 15 and 30 mVs-1). Internal series resistances of the supercapacitors were measured using the galvanostatic charge discharge curves also at room temperature. A maximum of 28 separators (δ=4200 μm) have been employed in this investigation. It has been shown that the ESR increases substantially with separator thickness (from 3.1 to 7.9 Ωcm2). The specific capacitance decreased somewhat with increasing separator thickness and scan rates (from 64 to 52 Fg-1; at 5 mVs-1). The microstructures of the electrode material have been investigated using scanning electron microscopy (SEM) and chemical microanalyses employing energy dispersive X-ray analysis (EDX). A compositional and morphological evaluation of these electrodes showed a very homogeneous microstructure.

Graphene oxide (GO) can be partially reduced to graphene-like sheets by removing the oxygen-containing groups and recovering the conjugated structure. In this work, the thermal reduction of GO powder has been carried out using back pumping vacuum pressures and investigated employing X-ray diffraction analysis. The experimental results of estimating the number of graphene layers on the reduced powder at various temperatures (200 – 1000 °C) have been reported. Electrical changes have been produced in a graphene oxide with the vacuum reduction process. This study has shown that the ideal processing temperature for reducing graphene oxide nanomaterial was about 400 °C. It has also been shown that at 600 °C the number of layers in the reduced nanomaterial increased. The internal series equivalent resistance (ESR) has been improved substantially with the vacuum thermal treatment even at temperatures above 400 °C. ESR was reduced from 95.0 to about 13.8 Ω cm2 with this processing. These results showed that the process can be applied to the reduction of graphene oxide to produce supercapacitor nanomaterials. The advantage of employing this method is that the processing is a straightforward and low cost thermal treatment that might be used for large amount of nanocomposite material.

This paper presents the results obtained from the hydrogenation and decrepitation of three LaNi-based alloys, La0.7Mg0.3Al0.3Mn0.4Co0.5Ni3.8, La0.7Mg0.3Al0.3Mn0.4Cu0.5Ni3.8and La0.7Mg0.3Al0.3Mn0.4Sn0.5Ni3.8, in the as-cast condition. The procedure for decrepitating the alloys to be used in the negative electrode of the batteries was carried out using a combination of various hydrogen pressures (2-9 bar) at room temperature. At 2 bar of H2it was revealed that Co, Cu and Sn have influence on the microstructures of the hydrogenated alloys and on the efficiency of hydrogen decrepitation. None of these alloys required thermal heating to activate and start the hydrogen absorption process. The decrepitated materials were characterized by scanning electron microscopy (SEM). The electrochemical measurements were performed using the tested negative electrode between two Ni (OH)2electrodes as a battery cell.

The addition of alloying elements on rare-earth permanent magnets is one of the methods used to improve the magnetic properties. This present work evaluates the influence of alloying elements such as Zr, Nb and Mo on the microstructure and magnetic properties of sintered Pr-FeCo-B based permanent magnets. The permanent magnets were produced by the conventional powder metallurgy route using powder obtained by hydrogen-decrepitation (HD) method from as cast alloys. In order to produce the magnet Pr16Fe66,9Co10,7B5,7Cu0,7 without alloying elements the mixture of alloys method was employed, mixing two compositions: Pr20Fe73B5Cu2 (33% w.t) and Pr14Fe64Co16B6 (67% w.t). With the purpose of evaluating the influence of the alloying elements, the Pr14Fe64Co16B6X0,1 (where X= Zr, Nb or Mo) (67% w.t) alloy was employed. The characterization of the alloys and the magnets was carried out using scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDXS) and the magnetic properties were measured using a permeameter. The magnet without any additions presented the highest intrinsic coercivity (μ0iHc = 748 KA.m-1) while the magnet with Nb addition presented higher remanence (Br = 1,04 T). The magnet with Zr addition presented the highest maximum energy product (BHmáx = 144 KJ.m-3), and the magnet with Mo addition showed the highest squareness factor (SF = 0,73).

In this paper, the effect of the grain size on sintered Nd-Fe-B based permanent magnets was investigated. In order, the magnets were produced by different milling times at 200 rpm and then vacuum sintered at 1373 K for 60 minutes followed by cooling outside the furnace. The magnets either produced by lower and higher milling times (30 and 75 minutes) exhibited lower remanence and coercivity, due the inhomogeneous distribution of the grain sizes. The magnet produced by intermediary milling time (45 minutes) exhibited the highest properties among all samples, with remanence of 1.06 T, coercivity of 891.3 KA.m-1, maximum energy product of 211 KJ.m3and a squareness factor equal 0.92.

Graphene has attracted significant interest because of its excellent electrical properties. However, a practical method for producing graphene on a large scale is yet to be developed. Graphene oxide (GO) can be partially reduced to graphene-like sheets by removing the oxygen-containing groups and recovering the conjugated structure. GO can be produced using inexpensive graphite as the raw material via cost-effective chemical methods. High vacuum and temperature (10−7 mbar and 1100°C, respectively) conditions are well-known to enable the preparation of reduced powder at the laboratory scale. However, a large-scale high vacuum reduction system that can be routinely operated at 10−7 mbar requires considerable initial capital as well as substantial operational and maintenance costs. The current study aims at developing an inexpensive method for the large-scale reduction of graphene oxide. A stainless steel vessel was evacuated to backing-pump pressure (10−2 mbar) and used to process GO at a range of temperatures. The reduction of GO powder at low vacuum pressures was attempted and investigated by X-ray diffraction and Fourier transform infrared spectroscopy. The experimental results of processing GO powder at various temperatures (200–1000°C) at relatively low pressures are reported. The microstructures of the processed materials were investigated using scanning electron microscopy and chemical microanalyses via energy dispersive X-ray analysis.

In recent years, extensive investigations have focused on the study and improvement of supercapacitor electrode materials. The electric devices produced with these materials are used to store energy over time periods ranging from seconds to several days. The main factor that determines the energy storage period of a supercapacitor is its self-discharge rate, i.e., the gradual decrease in electric potential that occurs when the supercapacitor terminals are not connected to either a charging circuit or electric load. Self-discharge is attenuated at lower temperatures, resulting in an increased energy storage period. This paper addresses the temperature-dependence of self-discharge via a systematic study of supercapacitors with nominal capacitances of 1.0 and 10.0 F at DC potentials of 5.5 and 2.7 V, respectively. The specific capacitances, internal resistances, and self-discharge characteristics of commercial activated carbon electrode supercapacitors were investigated. Using cyclic voltammetry, the specific capacitances were determined to be 44.4 and 66.7 Fg−1 for distinct carbon electrode supercapacitors. The self-discharge characteristics were investigated at both room temperature and close to the freezing point. The internal resistances of the supercapacitors were calculated using the discharge curves at room temperature. The microstructures of the electrode materials were determined using scanning electron microscopy.

Graphene (G) has been attracted great interest for its excellent electrical properties. However, the large-scale production of graphene is presently unfeasible. Graphene oxide (GO) can be (partly) reduced to graphene-like sheets by removing the oxygen-containing groups with the recovery of a conjugated structure. It can be produced using inexpensive graphite as raw material by cost-effective chemical methods. Although hydrogen (mixed with argon) at high temperature (1100°C) has been employed to reduce GO powder, the hydrogenation disproportionation desorption and recombination (HDDR) process in particular was unreported for this purpose. In the present work, attempts of reducing GO powder using the HDDR process have been carried out and investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy (FTIR). The experimental results of processing graphene oxide powder using unmixed hydrogen at moderate temperatures (about 850°C) and relatively low pressures (

This paper reports the results of investigation carried out to evaluate the corrosion resistance of tin and copper in as-cast alloys represented by two sequential series, first: La0.7Mg0.3Al0.3Mn0.4Co0.5-xSnxNi3.8 (x = 0.0, 0.1, 0.2, 0.3 and 0.5) and second: La0.7Mg0.3Al0.3Mn0.4Sn0.5-yCuyNi3.8 (y = 0.0, 0.1, 0.2, 0.3 and 0.5). Electrochemical methods, specifically, polarization curves have been employed in this study. Copper substitution yielded good overall performance of the alloys.

The effects of substituting Cu for Sn on the microstructure, hydrogen storage capacity of La0.7Mg0.3Al0.3Mn0.4Sn0.5−xCuxNi3.8 alloys (where X = 0.0, 0.1, 0.2, 0.3, and 0.5) alloys were investigated with X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and pressure-composition isotherms (PCIs). The alloys were mainly composed of three phases: LaNi5, MgNi2, and LaNiSn. However, the La0.7Mg0.3Al0.3Mn0.4Cu0.5Ni3.8 alloy (X = 0.5) exhibited a (La, Mg)Ni3 phase when studied with SEM. The PCI tests showed that increasing the Cu content increases the maximum hydrogen storage capacity.

The effects of substitution of Sn for Co on the microstructure, hydrogen storage and electrochemical discharge capacity of La 0.7 Mg 0.3 Al 0.3 Mn 0.4 Co 0.5– x Sn x Ni 3.8 ( x =0, 0.1, 0.2, 0.3 and 0.5) alloys were investigated using X-ray diffraction (XRD), pressure composition isotherm (PCT) and electrochemical discharge cycle. XRD, scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) tests showed that all of alloys are mainly composed of LaNi 5 and MgNi 2 phases, but when increasing the content of Sn in alloys, the LaNiSn phase appears and microstructure is refined. The PCT showed that increasing substitution of Sn for Co results in decrease of the maximum hydrogen storage capacity from 1.48% ( x =0) to 0.85% ( x =0.5). The electrochemical tests indicated that the maximum discharge capacity decreases from 337.1 mA·h/g ( x =0) to 239.8 mA·h/g ( x =0.5); however, the discharge capacity retention at the 100th cycle increases from 70.2% ( x =0) to 78.0% ( x =0.5).

Ti-13Nb-13Zr alloy produced via powder metallurgy was submitted to heat treatment under various conditions and the effects on microstructure and elastic modulus were investigated. Heat treatment was performed using temperatures above and below α/β transus combined with different cooling rates – furnace cooling and water quenching. Microstructure and phases were analyzed employing scanning electron microscopy and X-ray diffraction. Elastic Modulus was determined using a dynamic mechanical analyzer (DMA). The results indicated that α phase precipitation and elastic modulus values increased after heat treatment performed using temperature below α/β transus. However, when it was performed above α/β transus and using higher cooling rate, a decrease in elastic modulus was observed despite higher α phase precipitation, indicating that the microstructural modifications observed via SEM, due to the presence of martensitic α phase, influenced on elastic modulus values.

The microstructure and electrochemical properties of a La0.7Mg0.3Al0.3Mn0.4Co0.5Ni3.8 hydrogen storage alloy have been studied. The anode was prepared using a mixture of the ingot alloy in the as-cast state with carbon black and polytetrafluoroethylene (PTFE) as a binder. A Ni (OH)2 electrode was used as the cathode of the square-type test cell. A separator was used together with a 6M KOH electrolyte. Microstructure and phase composition of the alloy have been investigated using inductively coupled plasma atomic emission spectrometry (ICP-AES), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and X-ray diffraction analysis (XRD). A niobium-containing alloy has also been included for a comparison.

The preparation of negative electrodes for nickel-metal hydride (Ni-MH) batteries using a La0.7Mg0.3Al0.3Mn0.4Co0.5Ni3.8 alloy in the as-cast state has been carried out. The alloy was mechanically crushed (

A nickel-metal hydride (Ni-MH) rechargeable battery has been prepared using a La0.7Mg0.3Al0.3Mn0.4Co0.5Ni3.8 alloy as the negative electrode. The maximum discharge capacity of the La0.7Mg0.3Al0.3Mn0.4Co0.5Ni3.8 alloy has been determined (350 mAh/g). Using a high starting charging rate (2857 mAg-1) an efficiency of 49% has been achieved in the 4th cycle. The alloy and powders have been characterized by scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and X-ray diffraction (XRD).

Neste trabalho foi estudado as ligas La0,7-xMgx Pr0,3Al0,3Mn0,4Co0,5Ni3,8 (x = 0 a 0,7) como eletrodo negativo de baterias de níquel - hidreto metálico. A hidrogenação das ligas foi realizada com duas pressões de H2 (2 bar e 10 bar) e temperaturas (ambiente e 500°C). A capacidade de descarga das ba terias de níquel hidreto metálico foram analisadas pelo equipamento de testes elétricos ARBIN BT-4. As ligas, no estado bruto de fusão, foram analisadas por microscopia eletrônica de varredura (MEV), espectroscopia de energia dispersiva (EDS) e difração de Raios-X. Com o aumento da concentração de Mg nas ligas aumenta-se a capacidade de descarga, porém nota-se a diminuição a estabilidade cíclica das baterias. A capacidade de descarga máxima obtida foi para a liga Mg0,7Pr0,3Al0,3Mn0,4Co0,5Ni3,8 (60 mAh) e a bateria que apresentou a melhor performance foi La0,4Mg0,3Pr0,3Al0,3Mn0,4Co0,5Ni3,8 (53 mAh e 150 ciclos). A capacidade de absorção de hidrogênio diminui quando se adiciona Mg, não ocorrendo tal efeito para a liga Mg0,7Pr0,3Al0,3Mn0,4Co0,5Ni3,8. In this work were studied of La0.7-xMgx Pr0.3Al0.3Mn0.4Co0.5Ni3.8 (x = 0 and 0.7) alloys for negative electrodes of the nickel-metal hydride batteries. The hydrogenation of the alloys was performed varying pressing of H2 (2 and 10 bar) and temperature (room and 500°C). The discharge capacity of the nic kel-metal hydride batteries were analyzed in ARBIN BT- 4 electrical test equipment. The as-cast alloys were analyzed by scanning electron microscopy (SEM), energy disperse spectroscopy (EDX) and X-Ray diffraction. The increasing Mg addition in the alloy increases maximum discharge capacity but decrease cycle life of the batteries. The maximum discharge capacity was obtained with the Mg0.7Pr0.3Al0.3Mn0.4Co0.5Ni3.8 alloy (60 mAh) and the battery which presented the best performance was La0.4Mg0.3Pr0.3Al0.3Mn0.4Co0.5Ni3.8 alloy (53 mAh and 150 cycles). The H2 capability of absorption was diminished for increased Mg addition and no such effect occurs for Mg0.7Pr0.3Al0.3Mn0.4Co0.5Ni3.8 alloy.

The effects of substitution of Cu for Sn on the electrochemical discharge capacity performance of La0.7Mg0.3Al0.3Mn0.4Sn0.5−xCuxNi3.8 (x = 0.0, 0.1, 0.2, 0.3, and 0.5) negative electrode alloys were investigated. Results indicate that increasing Cu content enhanced electrochemical behavior by increasing the maximum discharge capacity from 239.8 mA· h/g (x = 0) to 305.2 mA· h/g (x = 0.5), the discharge capacity retention at the 100th cycle from 78.0% (x = 0) to 81.8% (x = 0.5), and the high rate dischargeability (HRD) from 25.7% (x = 0) to 80.6% (x = 0.5).

Neste trabalho, avaliou-se inicialmente o efeito da substituição de elementos em ligas à base de LaMgAlMnCoNi do tipo AB5 com adição de estanho (Sn) e cobre (Cu) em substituição ao cobalto (Co), para utilização em ligas absorvedoras de hidrogênio e em eletrodos negativos de baterias de Ni-HM. Avaliou-se a influência desta substituição na microestrutura do material. Notou-se que o aumento da concentração de estanho promove a formação da fase LaNiSn nas ligas, bem como a diminuição das duas fases principais: LaNi5 e (La,Mg)Ni3. Adicionalmente, utilizou-se o refinamento de Rietveld para quantificar as fases em cada composição. Posteriormente, propôs-se um estudo da absorção de hidrogênio. Notou-se que a liga com cobalto apresentou a melhor capacidade de absorção de hidrogênio. Ademais, verificou-se o comportamento destas ligas na capacidade de descarga, estabilidade cíclica e na alta taxa de descarga de baterias de Ni-HM. A maior capacidade de descarga medida foi para a liga de cobalto, atingindo 337,1 mAh/g. Notou-se, posteriormente uma melhora na estabilidade cíclica das baterias com o aumento do teor de cobre. Além disso, observou-se que a alta taxa de descarga apresenta melhores valores com a adição de cobre na composição. Por fim, avaliou-se o efeito da susceptibilidade a corrosão. Notou-se que o estanho promove um aumento na resistência à corrosão das ligas em eletrólito alcalino. In this work, it has firstly been evaluated the effect of tin (Sn) and copper (Cu) substituting cobalt (Co) in LaMgAlMnCoNi AB5-type alloys for use in hydrogen storage materials and negative electrodes of Ni-MH batteries. The influence of this substitution on the microstructure of these materials has been evaluated. It could be noted that increasing the tin concentration promotes the formation of LaNiSn phase and decrease of two main phases of these alloys: LaNi5 and (La,Mg)Ni3. Additionally, the Rietveld refinement has been evaluated to quantify phases in each composition. Subsequently, it has been proposed a study of the hydrogen absorption in these alloys. It could be observed that the cobalt alloy showed the best hydrogen absorption capacity. Moreover, the behavior of these alloys has been investigated in the discharge capacity, cyclic stability and high rate dischargeability of Ni-MH batteries. The highest discharge capacity has been measured for cobalt alloy, reaching 337.1 mAh/g. It has been noted, further improvement in the cyclic stability batteries with increasing copper content in the alloys. Furthermore, it has been observed that the high rate dischargeability has better values with the addition of copper in the composition. Finally, it has been evaluated the effect of susceptibility to corrosion. It has been noted that tin promotes an increase in corrosion resistance of the alloys in an alkaline electrolyte.

O presente trabalho descreve um processo atraente e verde para obtenção de nanocompósitos de rOG-Ni utilizando a radiação ionizante: radiação gama e feixe de elétrons. Os experimentos foram realizados, em meio aquoso, a temperatura e pressão ambiente e sem a geração de resíduos tóxicos e subprodutos indesejáveis. O OG foi esfoliado em água/isopropanol (1:1) e submetido à radiação gama nas doses de 20, 40 e 80 kGy e taxa de dose de 10 kGy/h para a obtenção do rOG. Para a síntese do rOG/Ni os experimentos foram realizados na presença de Ni(NH3)6Cl2. O rOG foi caracterizado por difração de Raios X (DRX), espectroscopia Raman e de fotoelétrons por Raios X (XPS) e o rOG-Ni por DRX e microscopia eletrônica de transmissão (MET). Os resultados de espectroscopia Raman e XPS confirmaram a formação do rOG e que o grau de redução foi proporcional ao aumento da dose aplicada sobre o óxido de grafeno. A morfologia do nanocompósito rOG-Ni foi avaliada por MET e pode-se observar nanopartículas de níquel uniformemente distribuídas sobre as folhas de rOG. Histogramas de tamanho médio de NPs indicaram que para a amostra sintetizadas por raios gama a 80 kGy, obteve-se nanopartículas menores quando comparada com a amostra irradiada a 40 kGy, sugerindo que, quanto maior a dose aplicada, menor o tamanho da nanopartícula formada. A comparar os resultados de DRX para o rOG-Ni obtido pelas duas técnicas de radiação ionizante, nas mesmas doses aplicadas, foi observado que para o nanocompósito sintetizado por radiação gama houve a redução do óxido de grafeno simultaneamente a formação das nanopartículas de níquel, enquanto que para o feixe de elétrons houve apenas a redução dos íons de níquel levando a formação da nanopartícula. Para estudo do comportamento eletroquímico, eletrodos do tipo screen printed electrode (SPE) foram modificados com o rOG e rOG-Ni sintetizados por radiação gama. Os voltamogramas cíclicos obtidos apresentaram um comportamento reversível para todas as amostras na presença de K4Fe(CN)6, e o valor da corrente de pico anódica (Ipa), mostrou-se diretamente proporcional ao aumento da dose aplicada sobre o nanomaterial em seu processo de redução. The present work describes an attractive and green process for obtaining rGO-Ni nanocomposites using ionizing radiation: gamma radiation and electron beam. The experiments were carried out in an aqueous medium, at ambient temperature and pressure and without the generation of toxic residues and undesirable products. The GO was exfoliated in water / isopropanol (1: 1) and subjected to gamma radiation at doses of 20, 40 and 80 kGy and a dose rate of 10 kGy / h to obtain the rGO. For the synthesis of rGO-Ni the experiments were carried out in the presence of Ni(NH3)6Cl2. The rGO was characterized by X ray diffraction (XRD), Raman spectroscopy and X ray photoelectron (XPS) and the rGO-Ni by XRD and transmission electron microscopy (TEM). The results of Raman and XPS spectroscopy confirmed a formation of the rGO and indicated the degree of reduction was proportional to the increase in the dose applied on graphene oxide. The morphology of the rGO-Ni nanocomposite was evaluated by TEM and it was observed nickel nanoparticles evenly distributed over the rGO sheets. Histograms of average size of NPs indicated for the sample synthesized by gamma rays at 80 kGy, smaller nanoparticles are obtained when compared to the sample irradiated at 40 kGy, suggesting that the higher the applied dose, the smaller the size of the nanoparticle formed. In comparing the results of XRD for rOG-Ni obtained by the two ionizing radiation techniques, at the same applied doses, it was observed that for the nanocomposite synthesized by gamma radiation there was a reduction of graphene oxide simultaneously with the formation of nickel nanoparticles, whereas for the electron beam only reduced nickel ions leading to the formation of the nanoparticle. To study the electrochemical behavior, the screen printed electrode (SPE) type electrodes were modified with the rGO and rGO-Ni synthesized by gamma radiation. The cyclic voltammograms showed a reversible behavior for all those in the presence of K4Fe(CN)6, and the value of the anodic peak current (Ipa), was directly proportional the increase in the dose applied on the nanomaterial in its reduction process.

O trabalho visa dispor sobre os resultados do estudo das características eletroquímicas de supercapacitores operando com eletrólito à base de líquido iônico de baixa toxicidade, considerando a influência da temperatura de operação e do potencial nominal máximo nas propriedades eletroquímicas de supercapacitores como indicadores da estabilidade eletroquímica do eletrólito empregado nestes dispositivos. Foi utilizado eletrodo comercial de carbono ativado, combinado em várias proporções molares, eletrólito a base de glicerol e KOH e sais de ChCl e K2CO3. Na primeira parte sem o revestimento do coletor de corrente acoplado com fio de níquel, e na segunda parte com revestimento do coletor de corrente acoplado com fio de platina com tinta sintética inoxidável e inerte. Os supercapacitores com eletrólitos de líquido iônico foram comparados com supercapacitores em eletrólitos que utilizam solução aquosa KOH e eletrólito orgânico, verificando a estabilidade e o comportamento dos supercapacitores entre a temperatura ambiente e a 80 °C. Ademais, foi avaliada a influência do tipo de eletrólito na capacidade de armazenamento e resistência interna em série (ESR) dos supercapacitores. As propriedades elétricas foram investigadas em um analisador eletrônico computadorizado com disponibilidade para testes de ciclos galvanostático e voltametria cíclica, determinando a capacitância específica e resistência interna. Foram realizados, também, microscopia eletrônica de varredura (MEV) e difração de raios X (DRX). As taxas de varredura de voltametria variaram de 1 a 30 mV s-1. Uma taxa de varredura mais baixa levou a uma capacitância específica mais alta com um potencial máximo aplicado de 2,1 V, tanto para os eletrólitos LIs à temperatura ambiente quanto para 80 °C. Além do aumento das concentrações molares dos eletrólitos e a elevação da temperatura do sistema para 80 °C em relação à temperatura ambiente levou a um maior valor de capacitância específica. No geral, o método do ciclo galvanostático teve um aumento na densidade de corrente elétrica, enquanto o tempo de carga e descarga diminuiu. The present work aims to provide on the results of the study of the electrochemical characteristics of supercapacitors operating with electrolyte based on low toxicity ionic liquid, considering the influence of operating temperature and maximum nominal potential on the electrochemical properties of supercapacitors as indicators of electrochemical stability of the electrolyte employed in these devices. Commercial activated carbon electrode was used, combined in various molar proportions, glycerol-based electrolyte with KOH, ChCl and K2CO3 salts. In the first part without the coating of the current collector coupled with nickel wire, and in the second part with coating of the current collector coupled with platinum wire with stainless and inert ink. Supercapacitors with ionic fluid electrolytes were compared with electrolyte supercapacitors using KOH aqueous solution and organic electrolyte, verifying the stability and behavior of supercapacitors between room temperature and 80 °C. Furthermore, the influence of electrolyte type on storage capacity and serial internal resistance (ESR) of supercapacitors was evaluated. The electrical properties were investigated in a computerized electronic analyzer with availability for tests of galvanostatic cycles and cyclic voltammetry, determining the specific capacitance and internal resistance. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) were also performed. Voltammetry scan rates ranged from 1 to 30 mV s-1. A lower scanning rate led to a higher specific capacitance with a maximum applied potential of 2.1 V, both for LIs electrolytes at room temperature and at 80 °C. In addition to the increase in the molar concentrations of electrolytes and the increase of the system temperature to 80 °C in relation to the ambient temperature led to a higher value of specific capacitance. In general, the galvanostatic cycle method had an increase in the density of electric current, the time of loading and discharge decreased.

A necessidade por energia elétrica tem impulsionado a pesquisa por fontes renováveis e sustentáveis para a geração de energia, como a energia solar. Neste sentido, as células solares sensibilizadas por corante (DSSC, do inglês Dye Sensitized Solar Cell) são promissoras por fornecer energia sobre qualquer intensidade luminosa. O óxido de zinco (ZnO) é um semicondutor do tipo n estudado para emprego nesses dispositivos por ser um material atóxico, barato e ambientalmente amigável, além de ter banda proibida de 3,7 eV. Este trabalho objetivou a obtenção de eletrodos de ZnO nanoestruturados seguindo os seguintes métodos: SILAR, do inglês, successive ionic layer adsorption and reaction, para obtenção da semente e; CBD, do inglês, chemical bath deposition, para crescimento da nanoestrutura. Para a síntese das nanoestruturas foi utilizado como precursores: acetato de zinco dihidratado, cloreto de zinco, sulfato de zinco heptahidratado e nitrato de zinco hexahidratado. Para cada precursor utilizado foram obtidos fotoanodos de filmes nanoestruturados com morfologias distintas com espessura da ordem de 10 µm, com orientação preferencial na direção do eixo basal e fotoanodos com o material particulado filtrado do banho químico. Estes fotoanodos foram caracterizados por microscopia eletrônica de varredura, microscopia de força atômica, fluorescência de raios X e difração de raio X. As DSSCs confeccionadas com fotoanodos de ZnO nanoestruturados mostraram que os mecanismos de transporte de cargas foram influenciados pela morfologia do ZnO. O material particulado originário dos sais de cloreto e nitrato de zinco apresentaram morfologia semelhante após a cominuição resultando em DSSCs semelhantes. A DSSC do pó de sulfato de zinco apresentou os melhores parâmetros elétricos e a maior eficiência (η = 0,71 ± 0,02 %). The increasing energy demand has motivated the research for renewable and sustainable sources for energy generation, such as solar energy. In this aspect, the dye sensitized solar cells (DSSC) are promising due its ability of providing energy over any light intensity. Zinc oxide (ZnO) is a well-studied n type semiconductor for use in these devices because it is a nontoxic material, inexpensive and environmental friendly, besides its physical characteristics, such as: band gap of 3,7 eV. The aim of this work was to synthesize ZnO nanostructured electrodes using the methods: Successive Ionic Layer Adsorption and Reaction (SILAR), for the seeds synthesis; and Chemical Bath Deposition (CBD), for the nanostructures growth. The nanostructures were synthesized using the precursors: zinc acetate dihydrate, zinc chloride, zinc sulfate heptahydrate and zinc nitrate hexahydrate. For each precursor, the photoanodes with distinct morphologies according to the zinc salt studied, 10 µm thick and with preferential orientation along the basal axis were obtained, and also photoanodes were obtained using the particulate material filtered from the chemical bath. The photoanodes were characterized by scanning electron microscopy, atomic force microscopy, X-ray fluorescence, and X-ray diffraction. The DSSC prepared using ZnO nanostructured photoanodes showed that the charge transport mechanism was influenced by the ZnO morphology. The particulate material from the chloride and nitrate zinc salts showed similar morphology after comminution, which resulted similar DSSCs. The DSSC produced using the de zinc sulfate powder presented the best electric parameters and it was the most efficient (η = 0,71 ± 0,02 %).

Neste trabalho, avaliou-se o efeito da substituição parcial do Ni pelos elementos Co, Cu e Sn, e do La e Mg pelo Pr em ligas do tipo AB5 para as ligas nominais La0,7Mg0,3Al0,3Mn0,4Cu0,5Ni3,8, La0,7Mg0,3Al0,3Mn0,4Co0,5Ni3,8 e La0,7Mg0,3Al0,3Mn0,4Sn0,5Ni3,8, La0,7Pr0,3Al0,3Mn0,4Co0,5Ni3,8, Pr0,7Mg0,3Al0,3Mn0,4Co0,5Ni3,8 sem e com tratamento térmico de 750° e 850°C por 9 e 16 horas. Estas ligas absorvedoras de hidrogênio foram utilizadas como material ativo em eletrodos negativos de baterias de Ni-HM. Avaliou-se a influência destas substituições e do tratamento térmico na microestrutura e nas propriedades eletroquímicas nas ligas. A substituição parcial do Ni pelo Co com o tratamento térmico de 750°C por 16 horas apresentou duas novas fases Al6Mn e PrCo13. Na substituição parcial do Ni pelo Sn formou a fase LaNi2Sn2 na liga. Utilizou-se caracterização de raios-X com refinamento de Rietveld para quantificar as fases em cada composição. Mediu-se a absorção de hidrogênio utilizando um Aparato Sieverts para obtenção das curvas PCT. Observou-se que as ligas La0,7Mg0,3Al0,3Mn0,4Co0,5Ni3,8 e La0,7Pr0,3Al0,3Mn0,4Co0,5Ni3,8 apresentaram as melhores capacidades de absorção de hidrogênio. Verificou-se o comportamento destas ligas na capacidade de descarga, estabilidade cíclica das baterias de Ni-HM. Comparando as ligas, a maior capacidade de descarga medida foi para a substituição parcial do Ni pelo Co, alcançando 406,1 mAh após o tratamento térmico de 850° C por 16 horas. A melhor capacidade de absorção obtida na analise de PCT, foi para a liga La0,7Pr0,3Al0,3Mn0,4Co0,5Ni3,8 com valor de H/M de 0,980. Também, foi avaliada uma correlação das propriedades eletroquímicas com a capacidade de absorção obtida na analise da curva PCT. In this work, it was evaluated the effect of the partial substitution of Ni by the elements Co, Cu and Sn and of the La and Mg by the Pr in type AB5 alloys to the nominal alloys La0,7Mg0,3Al0,3Mn0,4Cu0,5Ni3,8, La0,7Mg0,3Al0,3Mn0,4Co0,5Ni3,8, La0,7Mg0,3Al0,3Mn0,4Sn0,5Ni3,8, La0,7Pr0,3Al0,3Mn0,4Co0,5Ni3,8 and Pr0,7Mg0,3Al0,3Mn0,4Co0,5Ni3,8, as castting and with annealing treatment of 750 °C and 850 °C for 9 and 16 hours. These hydrogen-absorbing alloys were used as active material on negative electrodes of Ni-HM batteries. The influence of these substitutions and the annealing treatment on the microstructure and on the electrochemical properties in the alloys was evaluated. The partial substitution of Ni by Co with the annealing treatment of 750 °C for 16 hours presented two new phases Al6Mn and PrCo13. In the partial substitution of Ni by Sn formed the LaNi2Sn2 phase in the alloy. It was characterized by X-ray diffraction using Rietveld\'s refinement to quantify the phases in each composition. Hydrogen absorption was measured using the Sieverts apparatus to obtain the PCT curves. It was observed that the alloys La0,7Mg0,3Al0,3Mn0,4Co0,5Ni3,8 and La0,7Pr0,3Al0,3Mn0,4Co0,5Ni3,8, presented the best capacities of hydrogen absorption. The behavior of these alloys in the discharge capacity, the cyclic stability of the Ni-HM batteries, was verified. Comparing the alloys, the biggest discharge capacity measured was for the partial substitution of Ni by Co alloy, reaching 406.1 mAh after the annealing treatment of 850 °C for 16 hours. The finest absorption capacity obtained in the PCT analysis was for the La0,7Pr0,3Al0,3Mn0,4Co0,5Ni3,8 alloy with an H/M value of 0.980. Also, a correlation of the electrochemical properties with the absorption capacity obtained in the analysis of the PCT curve was evaluated.

O aumento da necessidade de armazenamento de energia trouxe aos capacitores eletroquímicos de dupla camada elétrica (supercapacitores) maiores proporções nas pesquisas. Com isto, a principal necessidade se tornou o aumento de sua capacidade (capacitância). Visando isto, o presente trabalho busca investigar o efeito do carbono ativado, matéria prima de eletrodos para os supercapacitores, tratado termicamente vácuo em diferentes temperaturas (200, 400, 600, 800 e 1000 °C) e por meio do processo HDDR,nas alterações das características elétricas destes produtos. Foram escolhidos dois eletrólitos de baixa toxidade em duas concentrações para salientar suas diferenças, sendo sulfato de sódio (1,0 mol L-1) e hidróxido de potássio (1,0 e 6,0 mol L-1). As medidas utilizadas para esta caracterização se basearam nos ensaios de voltametria cíclica e ciclos galvanostáticos, efetuados em um analisador computadorizado, determinando a capacitância especifica e resistência interna. Foram realizados, também, ensaios utilizando as seguintes técnicas: impedância, termogravimetria, adsorção de nitrogênio, microscopia eletrônica de varredura (MEV) e difração de raios X (DRX). The increased need for energy storage has brought the double-layer electrochemical capacitors (supercapacitors) larger proportions in research. With this, the main necessity became the increase of its capacity (capacitance). Aiming at this, the present work seeks to investigate the effect of activated carbon, electrode raw material for supercapacitors, heat treated vacuum at different temperatures (200, 400, 600, 800 and 1000 ° C) and through the HDDR process, in the alterations. electrical characteristics of these products. Two low-toxicity electrolytes were chosen at two concentrations to highlight their differences, sodium sulfate (1.0 mol L-1) and potassium hydroxide (1.0 and 6.0 mol L-1). The measurements used for this characterization were based on the cyclic voltammetry and galvanostatic cycles tests, performed in a computerized analyzer, determining the specific capacitance and internal resistance. Tests were also performed using the following techniques: impedance, thermogravimetry, nitrogen adsorption, scanning electron microscopy (SEM) and X-ray diffraction (XRD).

Nesse estudo foi sintetizado e caracterizado o óxido de grafeno (OG) a partir do método de Hummers modificado. O OG foi utilizado como suporte para nanopartículas de paládio para uso como eletrocatalisador em células a combustíveis abastecidas diretamente a etanol. O uso de carbono grafite como suporte de nanopartículas metálicas é deteriorado com mais rapidez, levando a diminuição do tempo de vida útil da célula a combustível. O objetivo principal foi a incorporação do paládio no óxido de grafeno via feixe de elétrons, e a comparação com o catalisador incorporado por via química, utilizando o borohidrato de sódio. Foram utilizadas técnicas de caracterização tais como: termogravimetria (TG), difração de raios-X (DRX), as espectroscopias de Raman e infravermelho com transformada de Fourier (FT-IR), microscopia de transmissão eletrônica (MET), Espectroscopia de fotoelétrons por raios- X (XPS) e estudos voltamétricos como a voltametria cíclica e cronoamperometria. Os resultados indicaram que para a dose de 288 kGy, houve a incorporação, porém, não foi suficiente para que houvesse a redução dos grupos oxigenados, estudos com o oxido de grafeno previamente reduzido via térmica e incorporado via feixe de elétrons foram comparados na mesma dose. In this study, graphene oxide (GO) was synthesized by the modified Hummers method and characterized. GO was used as support for palladium nanoparticles as an electrocatalyst on direct ethanol fuel cell (DEFC). One of the drawbacks using carbon graphite as a support for metal nanoparticles was because it deteriorates more quickly, leading to shortened fuel cell life. The main objective was the incorporation of Pd on the graphene oxide by the electron beam and was compared with the chemical incorporation, using sodium borohydride. Characterization techniques such as thermogravimetry (TG), X-ray diffraction (XRD), Raman spectroscopy and Fourier transform infrared (FT-IR), electron transmission microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and voltammetric studies such as cyclic voltammetry and chronoamperometry. The results indicated that at a dose of 288 kGy, there was an incorporation, however, it was not enough for there to be a decrease in the groups of oxygenates, studies with the graphene oxide downloaded through the thermal and through electron beams were compared in the same dose.

Neste estudo foi investigado o processo de redução térmica do óxido de grafeno em médio vácuo como uma rota viável de baixo custo econômico para obtenção do óxido de grafeno reduzido para aplicação em supercapacitores. O objetivo principal foi estudar a influência da temperatura de processamento no grau de redução do óxido de grafeno utilizando um sistema de vácuo com bomba mecânica de duplo estágio. O processamento constituiu na exposição do óxido de grafeno em várias temperaturas (200, 400, 600, 800 e 1000 °C) com pressão reduzida (10-2mbar) condição de médio vácuo. Foram utilizadas técnicas convencionais para caracterização dos materiais precursores e processados, tais como: microscopia eletrônica de varredura (MEV), difração de raios-X (DRX) e espectroscopia no infravermelho com transformada de Fourier (FTIR). Com os resultados deste estudo foi demostrado que é possível obter o óxido de grafeno reduzido utilizando um sistema de vácuo com bomba mecânica de duplo estágio e temperaturas de processamento superiores a 200°C. In this study the process of medium vacuum thermal reduction of the graphene oxide as a low cost route for obtaining reduced graphene oxide has been investigated. The main objective was to study the influence of the processing temperature on the degree of reduction of the graphene oxide using a vacuum system with two stage backing pump. The processing was carried out by exposing the graphene oxide at various temperatures (200, 400, 600, 800 e 1000 °C) with reduced pressure (10-2 mbar). Conventional techniques have been employed to the characterization of the starting and processed materials, such as: scanning electron microscopy (SEM), X-ray diffraction and Fourier transformed infrared spectroscopy (FTIR). With the results of this study it has been demonstrated that it is possible to obtain the reduced graphene oxide using a vacuum system with a two stage backing pump and processing temperatures superior to 200°C.

Neste trabalho foi proposto investigar as características de capacitores eletroquímicos de dupla camada elétrica (supercapacitores) utilizando como matéria prima um eletrólito biocompatível como rota viável de baixo custo econômico para obtenção de dispositivos eletrônicos para armazenamento de energia. O objetivo principal foi estudar a influência dos vários parâmetros de processamento nas características elétricas de supercapacitores à base de eletrólito neutro, utilizando, na preparação dos eletrodos oxido de grafeno reduzido via HDDR 400°C e o carbono ativado, também com baixa toxidade e impacto ambiental. O primeiro tópico consistiu na preparação de eletrólitos com diferentes concentrações para avaliar este parâmetro na curva de autodescarga dos supercapacitores. Alternativamente realizou-se a caracterização dos eletrodos preparados com oxido de grafeno reduzido via HDDR 400°C e carbono ativado por ensaios de voltametria cíclica em um analisador eletrônico computadorizado de supercapacitores, que resultou na determinação da capacitância específica do material precursor e das resistências internas. Foram utilizadas técnicas adicionais para caracterização dos materiais precursores e processados, tais como: microscopia eletrônica de varredura (MEV-EDS), difração de raios-X (DRX). On this work was proposed research the electrochemical double layer capacitors characteristics (supercapacitors) using an environmentally compatible electrolyte as viable low economic cost path to obtain electronics devices for energy storage. The mains objective was to study the influence of the various processing parameters on electrical characteristics of supercapacitors based in neutral electrolyte, using in the preparation the activated carbon and reduced graphene oxide HDDR 400°C, also with low toxicity and environmentally impact. The first topic consisted in the preparation of electrolytes with different concentrations to evaluate this parameter in the self-discharge curve of supercapacitors. Alternatively was made characterization experiments of the activated carbon electrodes and rGO HDDR 400°C by cyclic voltammetry essays in an electronic computerized analyzer of supercapacitors that resulted in the determination of the precursor material specific capacitance and internal resistances Was utilized additional technics for characterization of precursor materials such as scanning electron microscopy (MEV-EDX) and X-ray diffraction (DRX).