Mechanical behaviour of AISiC nano composites produced by Ball Milling and Spark Plasma Sintering

Neste trabalho foram produzidos nanocompósitos de AlSiC misturando alumínio puro com nano partículas de SiC com diâmetro de 45 – 55 nm, usando, de forma sequencial, a técnica da metalurgia do pó e a compactação por “ Spark Plasma Sintering”. O compósito obtido apresentava grãos com 100 nm de diâmetro, encontrandose as partículas de SiC localizadas, principalmente, nas fronteiras de grão. O nanocompósito sob a forma de provetes cilíndricos foi submetido a testes de compressão uniaxial e a testes de nanoindentação para analisar a influência das nanopartículas de SiC, da fração volúmica de ácido esteárico e do tempo de moagem, nas propriedades mecânicas do material. Para efeitos de comparação, utilizouse o comportamento mecânico do Al puro processado em condições similares e da liga de alumínio AA1050O. A tensão limite de elasticidade do nanocompósito com 1% Vol./Vol. de SiC é dez vezes superior à do AA1050. O refinamento de grão à escala nano constitui o principal mecanismo de aumento de resistência mecânica. Na realidade, o Al nanocristalino sem reforço de partículas de SiC, apresenta uma tensão limite de elasticidade sete vezes superior à da liga AA1050O. A adição de 0,5 % Vol./Vol. e de 1 % Vol./Vol. de SiC conduzem, respetivamente, ao aumento da tensão limite de elasticidade em 47 % e 50%. O aumento do tempo de moagem e a adição de ácido esteárico ao pó durante a moagem conduzem apenas a um pequeno aumento da tensão de escoamento. A dureza do material medida através de testes de nanoindentação confirmaram os dados anteriores. A estabilidade das microestruturas do alumínio puro e do nanocompósito AlSiC, foi testada através de recozimento de restauração realizado às temperaturas de 150 °C e 250 °C durante 2 horas. Aparentemente, o tratamento térmico não influenciou as propriedades mecânicas dos materiais, excepto do nanocompósito com 1 % Vol./Vol. de SiC restaurado à temperatura de 250 °C, para o qual se observou uma redução da tensão limite de elasticidade na ordem dos 13 %. No alumínio nanocristalino, a tensão de escoamento é controlada pelo efeito de HallPetch. As partículas de SiC, são segregadas pelas fronteiras do grão e não contribuem para o aumento de resistência mecânica segundo o mecanismo de Orowan. Alternativamente, as nanopartículas de SiC constituem um reforço das fronteiras do grão, impedindo o seu escorregamento e estabilizando a nanoestrutura. Deste modo, as propriedades mecânicas do alumínio nanocristalino e do nanocompósito de AlSiC poderão estar relacionadas com a facilidade ou dificuldade do escorregamento das fronteiras de grão, embora não seja apresentada prova explícita deste mecanismo à temperatura ambiente.

Ferroelectric : CNTs structures fabrication for advanced functional nano devices

This work is about the combination of functional ferroelectric oxides with Multiwall Carbon Nanotubes for microelectronic applications, as for example potential 3 Dimensional (3D) Non Volatile Ferroelectric Random Access Memories (NVFeRAM). Miniaturized electronics are ubiquitous now. The drive to downsize electronics has been spurred by needs of more performance into smaller packages at lower costs. But the trend of electronics miniaturization challenges board assembly materials, processes, and reliability. Semiconductor device and integrated circuit technology, coupled with its associated electronic packaging, forms the backbone of high-performance miniaturized electronic systems. However, as size decreases and functionalization increases in the modern electronics further size reduction is getting difficult; below a size limit the signal reliability and device performance deteriorate. Hence miniaturization of siliconbased electronics has limitations. On this background the Road Map for Semiconductor Industry (ITRS) suggests since 2011 alternative technologies, designated as More than Moore; being one of them based on carbon (carbon nanotubes (CNTs) and graphene) [1]. CNTs with their unique performance and three dimensionality at the nano-scale have been regarded as promising elements for miniaturized electronics [2]. CNTs are tubular in geometry and possess a unique set of properties, including ballistic electron transportation and a huge current caring capacity, which make them of great interest for future microelectronics [2]. Indeed CNTs might have a key role in the miniaturization of Non Volatile Ferroelectric Random Access Memories (NVFeRAM). Moving from a traditional two dimensional (2D) design (as is the case of thin films) to a 3D structure (based on a tridimensional arrangement of unidimensional structures) will result in the high reliability and sensing of the signals due to the large contribution from the bottom electrode. One way to achieve this 3D design is by using CNTs. Ferroelectrics (FE) are spontaneously polarized and can have high dielectric constants and interesting pyroelectric, piezoelectric, and electrooptic properties, being a key application of FE electronic memories. However, combining CNTs with FE functional oxides is challenging. It starts with materials compatibility, since crystallization temperature of FE and oxidation temperature of CNTs may overlap. In this case low temperature processing of FE is fundamental. Within this context in this work a systematic study on the fabrication of CNTs - FE structures using low cost low temperature methods was carried out. The FE under study are comprised of lead zirconate titanate (Pb1-xZrxTiO3, PZT), barium titanate (BaTiO3, BT) and bismuth ferrite (BiFeO3, BFO). The various aspects related to the fabrication, such as effect on thermal stability of MWCNTs, FE phase formation in presence of MWCNTs and interfaces between the CNTs/FE are addressed in this work. The ferroelectric response locally measured by Piezoresponse Force Microscopy (PFM) clearly evidenced that even at low processing temperatures FE on CNTs retain its ferroelectric nature. The work started by verifying the thermal decomposition behavior under different conditions of the multiwall CNTs (MWCNTs) used in this work. It was verified that purified MWCNTs are stable up to 420 ºC in air, as no weight loss occurs under non isothermal conditions, but morphology changes were observed for isothermal conditions at 400 ºC by Raman spectroscopy and Transmission Electron Microscopy (TEM). In oxygen-rich atmosphere MWCNTs started to oxidized at 200 ºC. However in argon-rich one and under a high heating rate MWCNTs remain stable up to 1300 ºC with a minimum sublimation. The activation energy for the decomposition of MWCNTs in air was calculated to lie between 80 and 108 kJ/mol. These results are relevant for the fabrication of MWCNTs – FE structures. Indeed we demonstrate that PZT can be deposited by sol gel at low temperatures on MWCNTs. And particularly interesting we prove that MWCNTs decrease the temperature and time for formation of PZT by ~100 ºC commensurate with a decrease in activation energy from 68±15 kJ/mol to 27±2 kJ/mol. As a consequence, monophasic PZT was obtained at 575 ºC for MWCNTs - PZT whereas for pure PZT traces of pyrochlore were still present at 650 ºC, where PZT phase formed due to homogeneous nucleation. The piezoelectric nature of MWCNTs - PZT synthesised at 500 ºC for 1 h was proved by PFM. In the continuation of this work we developed a low cost methodology of coating MWCNTs using a hybrid sol-gel / hydrothermal method. In this case the FE used as a proof of concept was BT. BT is a well-known lead free perovskite used in many microelectronic applications. However, synthesis by solid state reaction is typically performed around 1100 to 1300 ºC what jeopardizes the combination with MWCNTs. We also illustrate the ineffectiveness of conventional hydrothermal synthesis in this process due the formation of carbonates, namely BaCO3. The grown MWCNTs - BT structures are ferroelectric and exhibit an electromechanical response (15 pm/V). These results have broad implications since this strategy can also be extended to other compounds of materials with high crystallization temperatures. In addition the coverage of MWCNTs with FE can be optimized, in this case with non covalent functionalization of the tubes, namely with sodium dodecyl sulfate (SDS). MWCNTs were used as templates to grow, in this case single phase multiferroic BFO nanorods. This work shows that the use of nitric solvent results in severe damages of the MWCNTs layers that results in the early oxidation of the tubes during the annealing treatment. It was also observed that the use of nitric solvent results in the partial filling of MWCNTs with BFO due to the low surface tension (<119 mN/m) of the nitric solution. The opening of the caps and filling of the tubes occurs simultaneously during the refluxing step. Furthermore we verified that MWCNTs have a critical role in the fabrication of monophasic BFO; i.e. the oxidation of CNTs during the annealing process causes an oxygen deficient atmosphere that restrains the formation of Bi2O3 and monophasic BFO can be obtained. The morphology of the obtained BFO nano structures indicates that MWCNTs act as template to grow 1D structure of BFO. Magnetic measurements on these BFO nanostructures revealed a week ferromagnetic hysteresis loop with a coercive field of 956 Oe at 5 K. We also exploited the possible use of vertically-aligned multiwall carbon nanotubes (VA-MWCNTs) as bottom electrodes for microelectronics, for example for memory applications. As a proof of concept BiFeO3 (BFO) films were in-situ deposited on the surface of VA-MWCNTs by RF (Radio Frequency) magnetron sputtering. For in situ deposition temperature of 400 ºC and deposition time up to 2 h, BFO films cover the VA-MWCNTs and no damage occurs either in the film or MWCNTs. In spite of the macroscopic lossy polarization behaviour, the ferroelectric nature, domain structure and switching of these conformal BFO films was verified by PFM. A week ferromagnetic ordering loop was proved for BFO films on VA-MWCNTs having a coercive field of 700 Oe. Our systematic work is a significant step forward in the development of 3D memory cells; it clearly demonstrates that CNTs can be combined with FE oxides and can be used, for example, as the next 3D generation of FERAMs, not excluding however other different applications in microelectronics.

Compact dielectric-filled waveguide filters and diplexers

This paper presents electromagnetic simulations of dielectric-filled rectangular waveguide bandpass filter structures with microstrip to waveguide transitions as well as a diplexer based on such filters for modern wireless systems. The two bandpass filters have been designed and simulated at centre frequencies of 11.85 and 14.25 GHz, respectively. A significant size reduction is achieved through dielectric filling.

Compact filters using metal-dielectric inserts

A novel filter based on e-plane metal-dielectric insert in rectangular waveguide is proposed. Properties of the structure containing metallic septa, C- and I-shaped resonators placed in waveguide are investigated. Pseudo-elliptic cross-coupled filter with direct source-load coupling is designed, simulated and fabricated. Experimental results are presented to prove feasibility of the filter. Significant size reduction is achieved.

Ultra compact inline E-plane waveguide extracted pole bandpass filters

This letter presents an ultra compact extracted pole E-plane filter. The proposed structure can achieve up to 65% size reduction in comparison with a standard extracted pole filter designed at 9.5 GHz centre frequency with a 3% fractional bandwidth. The filter has been fabricated and tested using E-plane waveguide technology. Measurements on a fabricated filter confirm the accuracy of the design method.

Miniaturised sharp rejection bandpass filter with reconfigurable bandwidth for UWB applications

A novel, compact and highly selective microstrip bandpass filter with bandwidth reconfigurability for ultra-wideband (UWB) applications is presented. The proposed design uses stepped impedance resonator (SIR) for realization of bandpass filter (BPF) and employs a single varactor diode (BB135-NXP) for the purpose of reconfiguring bandwidth. Additionally, to improve the selectivity between passband edges, a cross-coupling between I/O feed lines is introduced which generated pairs of attenuation poles at each side of the passband. Measurements on a fabricated reconfigurable filter confirm the accuracy of the design procedure. Measured responses show good agreement with simulation. The proposed filter is able to achieve significant size reduction (8.5 mm × 7.1 mm excluding the feeding ports) as compared to the conventional bandpass filters with reconfigurable bandwidth.

Optimization process of polyester polymer mortars modified with recycled GFRP waste aggregates – application of factorial experiment design-

Glass fibre-reinforced plastics (GFRP), nowadays commonly used in the construction, transportation and automobile sectors, have been considered inherently difficult to recycle due to both: cross-linked nature of thermoset resins, which cannot be remolded, and complex composition of the composite itself, which includes glass fibres, matrix and different types of inorganic fillers. Presently, most of the GFRP waste is landfilled leading to negative environmental impacts and supplementary added costs. With an increasing awareness of environmental matters and the subsequent desire to save resources, recycling would convert an expensive waste disposal into a profitable reusable material. There are several methods to recycle GFR thermostable materials: (a) incineration, with partial energy recovery due to the heat generated during organic part combustion; (b) thermal and/or chemical recycling, such as solvolysis, pyrolisis and similar thermal decomposition processes, with glass fibre recovering; and (c) mechanical recycling or size reduction, in which the material is subjected to a milling process in order to obtain a specific grain size that makes the material suitable as reinforcement in new formulations. This last method has important advantages over the previous ones: there is no atmospheric pollution by gas emission, a much simpler equipment is required as compared with ovens necessary for thermal recycling processes, and does not require the use of chemical solvents with subsequent environmental impacts. In this study the effect of incorporation of recycled GFRP waste materials, obtained by means of milling processes, on mechanical behavior of polyester polymer mortars was assessed. For this purpose, different contents of recycled GFRP waste materials, with distinct size gradings, were incorporated into polyester polymer mortars as sand aggregates and filler replacements. The effect of GFRP waste treatment with silane coupling agent was also assessed. Design of experiments and data treatment were accomplish by means of factorial design and analysis of variance ANOVA. The use of factorial experiment design, instead of the one factor at-a-time method is efficient at allowing the evaluation of the effects and possible interactions of the different material factors involved. Experimental results were promising toward the recyclability of GFRP waste materials as polymer mortar aggregates, without significant loss of mechanical properties with regard to non-modified polymer mortars.

New end-use application for GFRP recyclates as reinforcement for concrete-polymer materials’

Glass fibre-reinforced plastics (GFRP), nowadays commonly used in the construction, transportation and automobile sectors, have been considered inherently difficult to recycle due to both: cross-linked nature of thermoset resins, which cannot be remolded, and complex composition of the composite itself, which includes glass fibres, matrix and different types of inorganic fillers. Presently, most of the GFRP waste is landfilled leading to negative environmental impacts and supplementary added costs. With an increasing awareness of environmental matters and the subsequent desire to save resources, recycling would convert an expensive waste disposal into a profitable reusable material. There are several methods to recycle GFR thermostable materials: (a) incineration, with partial energy recovery due to the heat generated during organic part combustion; (b) thermal and/or chemical recycling, such as solvolysis, pyrolisis and similar thermal decomposition processes, with glass fibre recovering; and (c) mechanical recycling or size reduction, in which the material is subjected to a milling process in order to obtain a specific grain size that makes the material suitable as reinforcement in new formulations. This last method has important advantages over the previous ones: there is no atmospheric pollution by gas emission, a much simpler equipment is required as compared with ovens necessary for thermal recycling processes, and does not require the use of chemical solvents with subsequent environmental impacts. In this study the effect of incorporation of recycled GFRP waste materials, obtained by means of milling processes, on mechanical behavior of polyester polymer mortars was assessed. For this purpose, different contents of recycled GFRP waste materials, with distinct size gradings, were incorporated into polyester polymer mortars as sand aggregates and filler replacements. The effect of GFRP waste treatment with silane coupling agent was also assessed. Design of experiments and data treatment were accomplish by means of factorial design and analysis of variance ANOVA. The use of factorial experiment design, instead of the one-factor-at-a-time method is efficient at allowing the evaluation of the effects and possible interactions of the different material factors involved. Experimental results were promising toward the recyclability of GFRP waste materials as aggregates and filler replacements for polymer mortar, with significant gain of mechanical properties with regard to non-modified polymer mortars.

Étude du potentiel cytotoxique des nanotubes de carbone simple-paroi chez les cellules épithéliales alvéolaires humaines A549

Il existe un grand intérêt pour le développement et les applications des nanotubes de carbone (NTC) car ils ont un énorme potentiel dans diverses applications industrielles. Cependant, leur dimension nanométrique et leur composition chimique peuvent constituer un risque sur la santé humaine. Les mécanismes responsables de la toxicité des NTC restent encore à définir. L’objectif de ce projet était de déterminer la toxicité potentielle de deux types de nanotubes de carbone simple-paroi (NTCSP): RN 000 et RN 003 chez une lignée cellulaire de pneumocytes de type II, les cellules A549. Méthodologie: Les essais MTS et PrestoBlue®, le test d’exclusion au bleu de trypan, la coloration HT-IP et l’Apoptotic Blebs ont été utilisés pour déterminer la toxicité potentielle de ces NTCSP. Résultats: Suite à une exposition de courte durée (24h), l’essai MTS a montré une diminution de la viabilité cellulaire significative de 20% pour [NTCSP] à 50 et 100 µg/ml et 74% pour [NTCSP] à 1000 µg/mL. Le PrestoBlue® a indiqué une mortalité cellulaire d’environ 45% et de 85% pour des concentration de 500 et 1000 µg/ml de NTCSP. Cependant, les données de l’essai d’exclusion du bleu de trypan ont montré que les NTCSP n’altèrent pas la viabilité cellulaire. L’absence d’une altération de la viabilité cellulaire a été confirmée avec la coloration HT-IP et l’Apoptotic Blebs. Cependant, l’interaction des NTCSP avec les cellules A549 a induit un changement de la morphologie cellulaire ; une diminution de la taille ainsi une augmentation de la structure interne des cellules A549. À une exposition à longue durée (72h), les données ont confirmé les résultats d’exposition à 24h. En effet, il n’y a de pas de mortalité cellulaire, mais une diminution de la prolifération cellulaire. En conclusion, notre étude indique que le RN 000 et le RN 003 interagissent avec les cellules A549 sans altérer leur viabilité, mais en induisant une dysfonction mitochondriale qui pourrait avoir plusieurs conséquences sur la fonction cellulaire.

Resonance Frequencies of Compact Microstrip Antenna

The arrow shaped microstrip antenna, which produces dual frequency dual polarisation operation with considera-ble size reduction compared to conventional patches has been reported [I]. These antennas provide greater area reduction and improved gain compared to drum shaped patches [2]. Prediction of the resonance frequency of drum shaped patches [3] and circular patches for broadband operation [4] are available in the literature. In this Letter, we propose empirical formulas for calculating the resonance frequencies of the arrow shaped microstrip antenna. These antennas can be employed for obtaining dual frequency with the same polarisation, bandwidth enhancement, circular polarisation etc. by varying its different parameters or by introducing slots. The proposed design equations provide an easier and simple way of predicting the resonant frequencies of these patches.

Single-feed dual-frequency dual-polarized slotted square microstrip antenna

A novel dual frequency dual-polarized square microstrip patch antenna embedded with a slot is presented. The proposed antenna offers tunability of the frequency ratio between the two frequencies by adjusting the slot dimensions. This configuration also provides a size reduction up to -51 and 35% for the two modes as compared to a square micro strip patch antenna

A Compact Novel Slot-Loaded Dual-Frequency H-Shaped Antenna

A novel compact single-layer dual frequency microstrip antenna which uses an H-shaped geometry with two U-shaped slots embedded near the radiation edges, is presented. By changing the design parameters, the lower and higher resonant frequencies can be controlled easily, and a range of frequency ratios (1.716-2.363) can be obtained in this design. For the two operating frequencies of the proposed antenna, the same polarization planes and broadside radiation patterns are achieved. Compared to the regular dualfrequency patch antenna, this antenna can realize a significant size reduction

A reconfiguration dual-frequency slot-loaded microstrip antenna controlled by pin diodes

A novel reconfigurable, single feed, dual frequency, dualpolarized operation of a hexagonal slot-loaded square mwrostrip antenna is presented in this paper. A pin diode incorporated in the slot is used to switch the two operating frequencies considerably, without significantly affecting the radiation characteristics and gain. The proposed antenna provides a size reduction up to 61% and 26% Jor the two resonating frequencies, compared to standard rectangular patches. This design also gives considerable bandwidth up to 3.3% and 4.27%, for the two frequencies with a low operating frequency ratio

Development of a varactor -controlled dual-frequency reconfigurable microstrip antenna

A new design for a compact electronically reconffgurable singlefeed dual frequency dual-polarized operation of a square-microstrip antenna capable of achieving tunable frequency ratios in the range 1.1 to 1.37 is proposed and experimentally studied. Varactor diodes inlegruted with the arms of the hexagonal slot and embedded in the square patch are used to tune the operating frequencies by applying reverse-bias voltage. The design has the advantage of size reduction up to 73.21% and 49.86% for the two resonant frequencies, respectively, as compared to standard rectangular patches. The antenna offers good bandwidth of 5.74% and 5.36% for the two operating frequencies. A highly simplified tuning circuitry without any transmission lines adds to the compactness of the design

A Compact Electronically Reconfigurable Dual Frequency Microstrip Antenna for L-Band Applications

A novel design of a computer electronically reconfigurable dual frequency dual polarized single feed hexagonal slot loaded microstrip antenna in L-band is introduced in this chapter. pin diodes are used to switch the operating frequencies considerably without much affecting the radiation characteristics and gain. the antenna can work with a frequency ratio varying in the wide range from 1.2 to 1.4. the proposed design has an added advantage of size reduction up to 72.21% and 46.84% for the two resonating frequencies compared to standard rectangular patches. the design also gives considerable bandwidth of up to 2.82% and 2.42 % for the operating frequencies.