ABSTRACT Radar absorbing materials (RAMs) are composites made with a polymeric matrix and an electromagnetic absorbing filler, such as carbon black (CB), silicon carbide (SiC) or manganese zinc ferrite (MnZn). To enhance their performances to attenuate an incident wave through reflection loss (RL), RAMs can be produced in multilayer structures. Usually, the RL analysis is done theoretically and experimentally validated with free space analysis. Here, it was demonstrated that multilayer structure can be designed and easily validated using rectangular waveguide, using a simpler setup and small samples. Three composites were produced using 2 wt% of CB (CB2), 40 wt% of SiC (SiC40) and 60 wt% of MnZn (MnZn60). They were characterized over the Ku-band and used to validate the multilayer structures, that were prepared by simply stacking each material inside the waveguide sample holder. One of the best results was obtained with structure SiC40+CB2 with 5.85 mm thickness, that presented a calculated RL of -21 dB at 17.8 GHz and a measured RL of -36 dB at the same frequency. In conclusion, using rectangular waveguide has been proven to be an easy, cheap, precise and fast approach to validate multilayer structures designs.

ABSTRACT This contribution reports the use of an organic gel, xerogel, as catalyst support for Cu. The xerogel was synthesized from the system tannin-formaldehyde at pH 3, using F-127 Pluronic as surfactant. The surface area values were higher than 900 m2/g even after the Cu (10%, wt) impregnation. The morphological analysis by SEM-FEG revealed the presence of spheres arranged in a tridimensional structure. XRD diffractograms showed the presence of CuO and Cu2O crystalline phases combined with the amorphous structure of the porous carbon. From XRD analysis it is possible to infer the Cu species are heterogeneously dispersed on the support with the co-existence of small and larger clusters, which is in agreement with Raman spectroscopy. Raman study also indicated a highly defect/disorder structure of the xerogel derivatives, ensuing the short-range structural order of the carbonic structure and oxygen groups decorating the carbon surface. XPS results corroborate with XRD and Raman results, detecting the presence of CuO and Cu2O. In addition to the mentioned Cu species, XPS also detected Cu0 which may be originated from the chemical interaction between the electron oxygen groups with the Cu precursor. The high surface area and the thermal stability (~ 300 ºC) of Cu/XCTF envisages its feasibly for relevant catalytic applications.

ABSTRACT Radar Absorbing Materials (RAMs) are composite materials able to attenuate an incident electromagnetic wave. Usually, RAMs are made of a polymeric matrix and an electromagnetic absorbent filler, such as silicon carbide or carbon black. Several materials have been investigated as potential fillers, aiming to improve the Reflection Loss (RL) and absorption bandwidth broadening. In this paper, a composite made with silicone rubber and biochar was investigated as a sustainable porous carbon made with biomass waste. Five different composites were characterized, composed of 1 - 5 wt.% of biochar in the silicone rubber. Although the RL of pure biochar composites is not significant, it was demonstrated here how a biochar composite can improve the RL of a RAM material when it is applied as a double-layer structure. While the RL of a ferrite-based RAM with 2.0 mm thickness reaches -28 dB, a combination of this RAM with biochar composite reaches ~ -60 dB with the same thickness. The double-layer structure with 2.3 mm thickness can have an absorption bandwidth of 2.95 GHz over the X-band frequency range, and a structure with 2.6 mm thickness can reach a RL of ~ -76 dB. This demonstrates a sustainable, cheaper, and lighter material application (i.e., biochar), which is successfully used in the development of high-efficient electromagnetic shield or sensors.

RESUMO Atualmente, existe uma demanda na busca por materiais com alta densidade de potência, longo ciclo de vida e baixo impacto ambiental que são em sua maioria utilizados para a produção de supercapacitores, sendo esses considerados fontes promissoras de energia para sistemas eletrônicos. Os tipos de materiais mais promissores para essa aplicação são os baseados em carbono, devido à sua flexibilidade, área superficial e boa estabilidade eletroquímica. Para a produção de materiais carbonosos, o principal precursor utilizado é a poliacrilonitrila (PAN) e suas variações a partir da adição de monômeros, como o acrilato de metila (MA). Geralmente, esses materiais são utilizados em formas de mantas, fios ou nanofibras produzidos a partir de processos de fiação e posteriormente carbonizados para gerar o material carbonáceo. Um dos processos de fiação que tem sido amplamente estudado para a obtenção de nanofibras de carbono é o processo de eletrofiação. Portanto, este trabalho apresenta os resultados obtidos do processo de carbonização de mantas eletrofiadas a partir de solução de PAN homopolímero (PANH) e PAN-co-acrilato de metila 6 % (PA6MA) com dimetilformamida (DMF) com o intuito de obter material para uso em supercapacitores. Os polímeros utilizados foram analisados por DSC para a obtenção dos valores relacionados a faixa de ciclização, sendo possível observar uma melhor estabilidade térmica relacionada as amostras de PAN6MA com faixa de temperatura de 240-312 °C e temperatura máxima do pico exotérmico de 292 °C. As mantas obtidas pelo processo de eletrofiação foram oxidadas a 235°C por 5min e carbonizadas a 900 °C por 5 min. As mantas obtidas, antes e após o processo de carbonização, foram analisadas por MEV apresentando fibras de superfície lisa, dispersas aleatoriamente e de dimensões nanométricas, sendo os valores de diâmetro aproximado de 219 nm para as nanofibras de carbono de PANH (NfcPANH) e 185 nm para as nanofibras de carbono de PAN6MA (NfcPAN6MA). As mantas carbonizadas foram analisadas pela técnica RAMAN e foi possível a obtenção de dados referentes a estrutura carbônica presente nas amostras, onde os valores obtidos demonstraram que as amostras de NfcPAN6MA apresentaram menor valor de grau de cristalinidade medida a partir da relação entre as bandas D e G conhecido como fator ID/IG, sendo o valor obtido igual a 1,06 para as NfcPNA6MA e 1,24 para as NfcPANH, isso demonstra uma maior presença de estruturas grafíticas cristalinas quando comparadas as amostras produzidas a partir da PANH. Para obtenção das características capacitivas foram realizados levantamento das curvas carga/ descarga por análise cronopotenciométrica, foi possível observar as melhores características relacionadas a capacitância específica e estabilidade de ciclagem em baixas correntes aplicadas para as amostras de PAN6MA com valores de capacitância específica de 270,9 F/g, densidade de energia de 30,0 Wh/kg e densidade de potência de 153,5 W/kg. Os resultados obtidos demonstraram que o material apresentou potencial para a aplicação proposta.

ABSTRACT Currently, there is a demand in the search for materials with high power density, long life cycle and low environmental impact that are mostly used fot the supercapacitors production, which are considered promising energy power for electronic systems. The most promising types of materials for this application are those based on carbon, due to their flexibility, surface area and good electrochemical stability. For the production of carbonaceous materials, the main precursor used is polyacrylonitrile (PAN) and its variations from the addition of monomers, such as methyl acrylate (MA). Generally, these materials are used in forms of blankets or yarns produced from spinning processes and later carbonized to generate the carbonaceous material. One of the spinning processes that has been widely studied for obtaining carbon nanofibers is the electrospinning process. Therefore, this paper presents the results obtained from the carbonization of electrospun blankets manufactured from solutions of polyacrylonitrile homopolymer (PANH) and poly (acrylonitrile-co-6 % methyl acrylate) (PAN6MA) combined with dimethylformamide in order to obtain material for use in supercapacitors. The polymers used were analyzed by DSC to obtain the values related to cyclization, by that were possible to observe a better thermal stability related to the samples of PAN6MA, with a temperature range of 240-312 ºC and maximum temperature of the exothermic peak of 292 °C. The electrospun mats were oxidized at 235°C per 5 min and carbonized at 90 °C per 5 min. Both pre-carbonization and post-carbonization mats were analyzed by SEM, showing fibers with smooth surface, randomly dispersion and nanometric size, with values of diameter of approximately 219 nm for PANH carbon nanofibers (NfcPANH) and 185 nm for PAN6MA carbon nanofibers (NfcPAN6MA). The carbonized mats were analyzed by RAMAN technique and it was possible to obtain the data related to the carbon structure present in the samples, where the obtained values showed that the mats manufactured from PAN6MA presented the lower value of degree of crystallinity measured from the relationship between bands D and G known as factor ID/IG, the value obtained being equal to 1.06 for NfcPAN6MA and 1.24 for NfcPANH, this shows a higher concentration of crystalline graphitic structures when compared with the samples produced from PANH. To obtain the capacitive characteristic, the load/discharge curves were surveyed by chronopotentiometric analysis, where it was possible to observe the best characteristics related to the specific capacity and low current cycling stability applied to the PAN - co- 6% methyl acrylate sample with specific capacity values of 270.9 F/g, energy density of 30.0 Wh/kg and power density of 153.5 W/kg. The results obtained demonstrated that the material presented potential for the proposed application.

RESUMO Compósitos poliméricos reforçados com fibras de carbono são materiais cada vez mais utilizados em diferentes segmentos industriais, em especial, os segmentos aeronáuticos e automobilísticos devido a sua elevada resistência mecânica e baixa massa específica. Desta forma, existe grande preocupação com o descarte e a reciclagem dos componentes que representam produtos de alto valor econômico agregado, principalmente fibras de carbono. O processo de pirólise tem sido um dos métodos de reciclagem de compósitos para recuperar as fibras de carbono a partir da degradação da matriz polimérica. No setor de energia, fibras de carbono são traduzidas como bons materiais de armazenamento de energia, por apresentar desejáveis características condutoras e capacitivas que potencializam sua aplicação como material de eletrodo em supercapacitores. Neste sentido, a proposta deste trabalho consiste em viabilizar o uso de fibras de carbono recicladas por pirólise de compósitos epóxi reforçado com fibras de carbono como material de eletrodo de supercapacitores e avaliar a influência dos tratamentos termoquímico e químico sobre suas propriedades capacitivas. Imagens FEG-MEV mostraram que as fibras de carbono foram praticamente limpas permanecendo um mínimo de carbono residual sobre a superfície. A área BET e as análises FTIR, Raman e de voltametria cíclica mostraram que os tratamentos termoquímico e químico realizados na FCP não contribuíram para melhorar a capacidade de armazenamento de cargas na interface eletrodo/eletrólito, pelo contrário, o tratamento químico levou a uma grande redução da capacidade da FCP no armazenamento de energia devido a incorporação de grupos OH e COOH. As curvas de carga/descarga evidenciam boa ciclabilidade e os valores de capacitância específica para a fibra de carbono reciclada de 34 Fg-1, densidade de potência de 37,6 Wkg-1 e densidade de energia de 4,7 Whkg-1encontram-se dentro da faixa para aplicações como eletrodos de supercapacitores.

ABSTRACT Carbon fiber reinforced polymeric composites are increasingly used materials in aeronautical and automotive industries, due to their excellent mechanical, chemical and electrical properties and low specific mass. In this way, there is a great concern regarding the components discard and recycling of the composites, which are considered as high economic value products to be wasted, mainly carbon fiber. The pyrolysis process has been one of the methods of recycling composites to recover carbon fibers from the degradation of the polymer matrix. In energy sector, carbon fibers are known as good energy storage materials due to adequate conducting and capacitive properties as supercapacitor electrodes. In this sense, the purpose of this work is to enable the use of recovered carbon fibers frompyrolysis of carbon fiber epoxy composites as electrode material for supercapacitors and to evaluate the influence of thermochemical and chemical treatments on their capacitive properties. FEG-MEV images showed that the carbon fibers were practically clean with a minimum of residual carbon remaining on the surface. The BET area and FTIR, Raman and cyclic voltammetry analyzes showed that thermochemical and chemical treatments carried out at the FCP did not contribute to improving the charge storage capacity at the electrode/ electrolyte interface. On the contrary, the chemical treatment led to a great reduction on energy storage capacity due to the incorporation of OH and COOH groups. The charge/discharge curves show good cycling and the specific capacitance values for the recycled carbon fiber of 34 Fg-1, power density of 37,6 Wkg-1 and energy density of 4,7 Whkg-1 are within range for applications such as supercapacitor electrodes.

ABSTRACT Carbon material is the largest material used as electrode on advanced energy storage devices. The modern lifestyle requires more energy, consequently, more smart energy use and efficient devices are needed. The constant evolution of materials technologies looking for green material and renewable raw material, that have minimal impact on the environment, is one of the most important subjects studied in recent years. The scientific and industry community are paying more attention to new forms of carbon such as nanotubes, graphene, and activated carbon fiber. The purpose of this work is to convert human hair into a hollow carbon filament to be used as a supercapacitor electrode. The human hair needs 3 stages to be converted into carbon filament: textile manufacture, oxidation, and carbonization. The electrochemical behavior was analyzed in a three-electrode electrochemical cell system with 2 M of H2SO4 electrolyte medium. The behavior of the electrode was characterized electrochemically by galvanostatic charge/discharge curves, cyclic voltammetry, and electrochemical impedance spectroscopy, showing 163 F g-1 of a maximum value of specific capacitance.

In this manuscript, the electromagnetic wave absorption properties of sustainable porous carbon composites were evaluated over the X-band frequency range (8.2 - 12.4 GHz). The porous carbon material was made from the byproduct of cellulose production and was used as additive on the development of radar absorbing material (RAM) composites. These porous carbon materials have different characteristics, such as porosity size (180 µm < Ø1 < 250 µm and 425 µm < Ø2 < 500 µm) and particle size (ϕ1 < 250 µm and 250 µm < ϕ2 < 425 µm). Composite materials were also studied as frequency selective surface (FSS) structures. It was shown how complex permittivity and reflection loss (RL) can be manipulated over the frequency range using FSS structure. While regular RAM presented RL of 19 dB at ~11.8 GHz, FSS structure presented a RL of 19 dB shifted to 12.4 GHz regarding the same carbon porous material (with particles between 250 and 425 µm and porosity between 180 and 250 µm). It was demonstrated here the potential use of sustainable porous carbon as RAM, and how FSS structure can be used to tune the frequency of the RL maximum peak.

The main challenge for the development of a high efficiency supercapacitor is the electrode material. Developing electrode materials with high specific electrical capacitance and low electrical resistance enables an increase in the energy accumulated in the device. In addition, it is expected that the electrode material presents a simple procedure for preparation having low production cost and being environmentally friendly. This work is based on the deposition of silver nanoparticles on activated carbon felt (Ag@ACF) as a supercapacitor electrode. The samples were characterized by field emission gun scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy and textural analysis. Supercapacitor behavior was evaluated by galvanostatic charge-discharge curves, cyclic voltammetry and electrochemical impedance spectroscopy using a symmetrical two-electrode Swagelok type cell, and three different aqueous solution electrolytes: 2 M H2SO4, 6 M KOH and 1 M Na2SO4. Ag@ACF presented a high specific capacitance in KOH, about 170 F g-1, which makes it an interesting material for supercapacitor electrodes and it showed good specific electrical capacitance, low resistance and high cyclability.

Abstract The aim of this work is to follow the structural variations of polyaniline (PAni) obtained by chemical oxidation on a pre-pilot scale, with different reaction times. Synthesis of PAni is well known, but when it is carried out on a pre-pilot scale, several factors can lead to structural changes and understanding these changes is important to improve controls on the synthesis process. The polymers formed were characterized by spectroscopic techniques (Raman spectroscopy, Fourier Transform Infrared - FTIR and UV-Visible). Degree of oxidation and yield were calculated for each reaction time. The analysis by FTIR, the calculated degree of oxidation and the yield showed significant changes in polymer structure at reaction times of 65 and 80 min. This result was attributed to the excessive oxidation of PAni, with the breaking of its polymer chain. The changes observed in the structure of PAni gave subsidies to the optimization of the process of obtaining polyaniline by chemical synthesis.

The evolution of TiO2 nanotubular morphology, synthesized in a mixture of fluorinated ethylene glycol and glycerol electrolyte, was studied as a function of the anodization time. The samples were characterized by FEG-SEM, XRD, XPS, UV-Vis and EIS. The formation of single-or double-walled TiO2 nanotube structure can be efficiently controlled by the anodization time. For anodization times less than 30 minutes, a compact oxide layer is formed, followed by double-walled nanotube formation up to 120 minutes and single-walled nanotubes up to 240 minutes. XPS analyses show that the samples obtained with short anodization time have a high carbon content and oxygenated surface species compared to the longer-time anodized sample; however, binding energy peaks for Ti 2p remained invariant. The performances of TiO2 nanotubular photoelectrodes were evaluated in photoelectrochemical water splitting where TiO2 nanotubes anodized for 120 minutes presented the best performance that was related to their optimal morphology and charge transportation.