ABSTRACT Currently, the presence of spurious microwave radiation is increasing in the environment, which has caused concern due to possible health problems in living beings and electromagnetic interference in electronic systems. To control this problem, studies in the materials area are taking place, aiming to attenuate the spurious radiation and meet requirements of good performance in broadband, low cost and low weight. The present work aimed to study Cu and Ni nanometric films with thicknesses of 65 and 200 nm, deposited on polyethylene terephthalate substrate by magnetron sputtering. Scanning electron microscopy with a field emission gun (FEG-SEM) showed that the films produced have different morphological textures, due to the parameters used in the sputtering process and also the free energy of metals. Impedance spectroscopy measurements showed that the films have low conductivity values, due to the metallic oxides formed on the film surfaces, confirmed by X-ray diffraction, and also to the presence of defects. Electromagnetic characterization (8.2 – 12.4 GHz) showed that the Cu and Ni thin films had low performance, except the Ni_200 nm film, which showed a total shielding efficiency of about 30% in broadband. This result is promising considering the nanometric thickness of the Ni film.

The great technological advancement in wireless communication systems and devices generated the problem of electromagnetic pollution. Developing lightweight, sustainable, and low-cost materials is necessary to minimize electromagnetic pollution. A sustainable porous carbon (PC) absorber material was obtained from the crude black liquor by a simple and low-cost synthesis, and combined with carbon nanotube (CNT), presenting excellent microwave attenuation results. The PC absorber at 20 wt.% filling ratio exhibited an intense reflection loss of ‑35.7 dB at 15.5 GHz, and bandwidth of 1.15 GHz for a thickness of 5.90 mm. By adding 0.2 wt.% of CNT, the reflection loss was -34.6 dB at 17.9 GHz, and a bandwidth of 1.54 GHz for 4.90 mm. The study reveals that the combination of PC and CNT improves the attenuation capacity, allows adjustment in the frequency range of the attenuation peak, and promotes thickness reduction. The results obtained allow us to advance studies in developing high-performance, sustainable, and low-cost microwave-absorbing materials.

This study aimed to synthesize a composite material composed of bio-based, porous carbon matrix and Cu nanoparticles through a simple, low-cost, and environmentally friendly method. Concentrated Kraft black liquor was used as a carbon precursor, and Cu nanoparticles were homogeneously deposited on the carbon matrix using electrochemical deposition. The textural properties determined using N2 isotherms indicated increased surface area of a carbon matrix with a micro-mesoporous structure. Voltammetric tests demonstrated that the composite exhibited catalytic properties for electrochemical CO2 reduction. Compared to the bio-based, porous carbon sample (C matrix), the bio-based carbon electrode electrochemically decorated with Cu nanoparticles (C–Cu composite) exhibited increased current values of approximately 2.4 times, a potential shift of approximately 90 mV, and an onset potential of −1.02 V, under CO2 saturation.

Abstract Carbonaceous porous materials are strong candidates for producing low-cost, lightweight, and sustainable electromagnetic (EM) absorbing materials. This work investigates the production of radar-absorbing materials (RAM) by a simple method. Sustainable carbon xerogel (CX) was synthesized from tannin, a biosourced molecule. CX and commercial carbon nanotube (CNT) were embedded in a silicone matrix at proportions of 10 and 15 wt.% of CX and 0.1 wt.% of CNT to produce flexible composites. The morphology and structure of the carbonaceous materials were evaluated by field-emission scanning electron microscopy (FEG-SEM), Raman spectroscopy, X-ray diffraction (XRD), textural properties by N2 adsorption-desorption isotherms, and mercury porosimetry. The electromagnetic characterization of the composites was analyzed by a vector network analyzer (VNA) in the Ku-band. The results demonstrated that an increased concentration of CX in the composite improved reflection loss reaching -43.19 dB at 13.79 GHz.

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 Este trabalho apresenta as propriedades eletromagnéticas de um Material Absorvedor de Radiação Eletromagnética (MARE) feito a partir de Carbeto de Silício (SiC) e Negro de Fumo (NF) como aditivos. O compósito SiC/NF foi produzido utilizando 70 %(m/m) de matriz de silicone, e variando as concentrações do aditivo em 3 %(m/m), 2 %(m/m) e 1 %(m/m) de NF com 27 %(m/m), 28 %(m/m) e 29 %(m/m) de SiC, respectivamente. A estrutura química e a morfologia das partículas de SiC e NF foram analisadas através de espectroscopia Raman e Microscopia Eletrônica de Varredura (MEV). As propriedades dielétricas dos MAREs foram obtidas por meio do analisador de rede vetorial na faixa de frequência de 12,4 a 18,0 GHz. Os resultados de refletividade mostraram que o compósito SiC/NF com 1 %(m/m) de NF apresentou a melhor absorção de radiação eletromagnética, chegando a -47,9 dB em 16,8 GHz com uma amostra de aproximadamente 5,5 mm de espessura.

ABSTRACT Este trabalho apresenta as propriedades eletromagnéticas de um Material Absorvedor de Radiação Eletromagnética (MARE) feito a partir de Carbeto de Silício (SiC) e Negro de Fumo (NF) como aditivos. O compósito SiC/NF foi produzido utilizando 70 %(m/m) de matriz de silicone, e variando as concentrações do aditivo em 3 %(m/m), 2 %(m/m) e 1 %(m/m) de NF com 27 %(m/m), 28 %(m/m) e 29 %(m/m) de SiC, respectivamente. A estrutura química e a morfologia das partículas de SiC e NF foram analisadas através de espectroscopia Raman e Microscopia Eletrônica de Varredura (MEV). As propriedades dielétricas dos MAREs foram obtidas por meio do analisador de rede vetorial na faixa de frequência de 12,4 a 18,0 GHz. Os resultados de refletividade mostraram que o compósito SiC/NF com 1 %(m/m) de NF apresentou a melhor absorção de radiação eletromagnética, chegando a -47,9 dB em 16,8 GHz com uma amostra de aproximadamente 5,5 mm de espessura.

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.

ABSTRACT The electromagnetic properties of Carbon-Graphene Xerogel (CGX), Flaky graphite (GR) and Nickel-Zinc ferrite (FeNiZn) composites in polystyrene (PS) matrix were studied in the X-Band range (8.2 – 12.4 GHz). In this work the Expanded Polystyrene (EPS) waste material was processed into polystyrene through the recycling of EPS. The polystyrene obtained was utilized as dielectric matrix, mainly because PS is a well-known organic polymer that presents low dielectric loss and light weight, which contribute to applications in composites for the aerospace field. In order to produce the final composite specimens, the CGX additive was previously synthesized through a sustainable method that employed the use of waste from the paper and pulp industry (black liquor). Afterwards, the morphological and structural analysis were made through Scanning Electron Microscope (SEM) and Raman Spectrometer, respectively. On the other hand, the magnetic ferrite material, FeNiZn, was obtained for the composite production through calcination, whereas the GR utilized was commercially obtained. It was observed that the increase of CGX and GR influenced on the increase of the Complex Permittivity, and that 10 wt% CGX + 50wt% FeNiZn composite sample demonstrated an absorption peak at 10.5 GHz. The results are relevant concerning the recycling of EPS waste through its use as dielectric matrix, thus developing greener and low-weight composite materials to be used in microwave applications.

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.