Search results for: 1D nanostructured polyaniline

Authors: Yeidy Sorani Montenegro Camacho, Samir Bensaid, Nunzio Russo, Debora Fino

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LiFeO2 nano-powders were prepared via solution combustion synthesis (SCS) method and were used as carbon gasification catalyst in a reduced atmosphere. The gasification of soot with CO2 and H2O in the presence of CO and H2 (syngas atmosphere) were also investigated under atmospheric conditions using a fixed-bed micro-reactor placed in an electric, PID-regulated oven. The catalytic bed was composed of 150 mg of inert silica, 45 mg of carbon (Printex-U) and 5 mg of catalyst. The bed was prepared by ball milling the mixture at 240 rpm for 15 min to get an intimate contact between the catalyst and soot. A Gas Hourly Space Velocity (GHSV) of 38.000 h-1 was used for the tests campaign. The furnace was heated up to the desired temperature, a flow of 120 mL/min was sent into the system and at the same time the concentrations of CO, CO2 and H2 were recorded at the reactor outlet using an EMERSON X-STREAM XEGP analyzer. Catalytic and non-catalytic soot gasification reactions were studied in a temperature range of 120°C – 850°C with a heating rate of 5 °C/min (non-isothermal case) and at 650°C for 40 minutes (isothermal case). Experimental results show that the gasification of soot with H2O and CO2 are inhibited by the H2 and CO, respectively. The soot conversion at 650°C decreases from 70.2% to 31.6% when the CO is present in the feed. Besides, the soot conversion was 73.1% and 48.6% for H2O-soot and H2O-H2-soot gasification reactions, respectively. Also, it was observed that the carbon gasification in mixed atmosphere, i.e., when simultaneous carbon gasification with CO2 and steam take place, with H2 and CO as co-reagents; the gasification reaction is strongly inhibited by CO and H2, as well has been observed in single atmospheres for the isothermal and non-isothermal reactions. Further, it has been observed that when CO2 and H2O react with carbon at the same time, there is a passive cooperation of steam and carbon dioxide in the gasification reaction, this means that the two gases operate on separate active sites without influencing each other. Finally, despite the extreme reduced operating conditions, it has been demonstrated that the 32.9% of the initial carbon was gasified using LiFeO2-catalyst, while in the non-catalytic case only 8% of the soot was gasified at 650°C.

Keywords: soot gasification, nanostructured catalyst, reducing environment, syngas

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Authors: Mohannad Mayyas, Farshid Pahlevani, Veena Sahajwalla

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Automotive shredder residue (ASR) is an industrial waste, generated during the recycling process of End-of-life vehicles. The large increasing production volumes of ASR and its hazardous content have raised concerns worldwide, leading some countries to impose more restrictions on ASR waste disposal and encouraging researchers to find efficient solutions for ASR processing. Although a great deal of research work has been carried out, all proposed solutions, to our knowledge, remain commercially and technically unproven. While the volume of waste materials continues to increase, the production of materials from new sustainable sources has become of great importance. Advanced ceramic materials such as nitrides, carbides and borides are widely used in a variety of applications. Among these ceramics, a great deal of attention has been recently paid to Titanium nitride (TiN) owing to its unique characteristics. In our study, we propose a new sustainable approach for ASR management where TiN nanoparticles with ideal particle size ranging from 200 to 315 nm can be synthesized as a by-product. In this approach, TiN is thermally synthesized by nitriding pressed mixture of automotive shredder residue (ASR) incorporated with titanium oxide (TiO2). Results indicated that TiO2 influences and catalyses degradation reactions of ASR and helps to achieve fast and full decomposition. In addition, the process resulted in titanium nitride (TiN) ceramic with several unique structures (porous nanostructured, polycrystalline, micro-spherical and nano-sized structures) that were simply obtained by tuning the ratio of TiO2 to ASR, and a product with appreciable TiN content of around 85% was achieved after only one hour nitridation at 1550 °C.

Keywords: automotive shredder residue, nano-ceramics, waste treatment, titanium nitride, thermal conversion

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Authors: Vishnu V. Pillai, Sunil P. Lonkar, Akhil M. Abraham, Saeed M. Alhassan

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An effectual technology for wastewater treatment is a great demand now in order to encounter the water pollution caused by organic pollutants. Photocatalytic oxidation technology is widely used in removal of such unsafe contaminants. Among the semi-conducting metal oxides, robust and thermally stable TiO2 has emerged as a fascinating material for photocatalysis. Enhanced catalytic activity was observed for nanostructured TiO2 due to its higher surface, chemical stability and higher oxidation ability. However, higher charge carrier recombination and wide band gap of TiO2 limits its use as a photocatalyst in the UV region. It is desirable to develop a photocatalyst that can efficiently absorb the visible light, which occupies the main part of the solar spectrum. Hence, in order to extend its photocatalytic efficiency under visible light, TiO2 nanoparticles are often doped with metallic or non-metallic elements. Non-metallic doping of TiO2 has attracted much attention due to the low thermal stability and enhanced recombination of charge carriers endowed by metallic doping of TiO2. Amongst, sulfur doped TiO2 is most widely used photocatalyst in environmental purification. However, the most of S-TiO2 synthesis technique uses toxic chemicals and complex procedures. Hence, a facile, scalable and environmentally benign preparation process for S-TiO2 is highly desirable. In present work, we have demonstrated new and facile solid-state reaction method for S-TiO2 synthesis that uses abundant elemental sulfur as S source and moderate temperatures. The resulting nano-sized S-TiO2 has been successfully employed as visible light photocatalyst in methylene blue dye removal from aqueous media.

Keywords: ecofriendly, nanomaterials, methylene blue, photocatalysts

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Authors: Ainouna Bouziane

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The ability of Electron Tomography to recover the 3D structure of catalysts, with spatial resolution in the subnanometer scale, has been widely explored and reviewed in the last decades. A variety of experimental techniques, based either on Transmission Electron Microscopy (TEM) or Scanning Transmission Electron Microscopy (STEM) have been used to reveal different features of nanostructured catalysts in 3D, but High Angle Annular Dark Field imaging in STEM mode (HAADF-STEM) stands out as the most frequently used, given its chemical sensitivity and avoidance of imaging artifacts related to diffraction phenomena when dealing with crystalline materials. In this regard, our group has developed a methodology that combines image denoising by undecimated wavelet transforms (UWT) with automated, advanced segmentation procedures and parameter selection methods using CS-TVM (Compressed Sensing-total variation minimization) algorithms to reveal more reliable quantitative information out of the 3D characterization studies. However, evaluating the accuracy of the magnitudes estimated from the segmented volumes is also an important issue that has not been properly addressed yet, because a perfectly known reference is needed. The problem particularly complicates in the case of multicomponent material systems. To tackle this key question, we have developed a methodology that incorporates volume reconstruction/segmentation methods. In particular, we have established an approach to evaluate, in quantitative terms, the accuracy of TVM reconstructions, which considers the influence of relevant experimental parameters like the range of tilt angles, image noise level or object orientation. The approach is based on the analysis of material-realistic, 3D phantoms, which include the most relevant features of the system under analysis.

Keywords: electron tomography, supported catalysts, nanometrology, error assessment

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Authors: Jingcheng Ma, Patricia B. Weisensee, Young H. Shin, Yujin Chang, Junjiao Tian, William P. King, Nenad Miljkovic

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Water droplet impact on surfaces is a ubiquitous phenomenon in both nature and industry. The transfer of mass, momentum and energy can be influenced by the time of contact between droplet and surface. In order to reduce the contact time, we study the influence of substrate motion prior to impact on the dynamics of droplet recoil. Using optical high speed imaging, we investigated the impact dynamics of macroscopic water droplets (~ 2mm) on rigid nanostructured superhydrophobic surfaces vibrating at 60 – 300 Hz and amplitudes of 0 – 3 mm. In addition, we studied the influence of the phase of the substrate at the moment of impact on total contact time. We demonstrate that substrate vibration can alter droplet dynamics, and decrease total contact time by as much as 50% compared to impact on stationary rigid superhydrophobic surfaces. Impact analysis revealed that the vibration frequency mainly affected the maximum contact time, while the amplitude of vibration had little direct effect on the contact time. Through mathematical modeling, we show that the oscillation amplitude influences the possibility density function of droplet impact at a given phase, and thus indirectly influences the average contact time. We also observed more vigorous droplet splashing and breakup during impact at larger amplitudes. Through semi-empirical mathematical modeling, we describe the relationship between contact time and vibration frequency, phase, and amplitude of the substrate. We also show that the maximum acceleration during the impact process is better suited as a threshold parameter for the onset of splashing than a Weber-number criterion. This study not only provides new insights into droplet impact physics on vibrating surfaces, but develops guidelines for the rational design of surfaces to achieve controllable droplet wetting in applications utilizing vibration.

Keywords: contact time, impact dynamics, oscillation, pear-shape droplet

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Authors: Zineb Kassab, Nassima El Miri, A. Aboulkas, Abdellatif Barakat, Mounir El Achaby

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Recently, more attention has been given to biopolymers with a focus on sustainable development and environmental preservation. Following this tendency, the attempt has been made to replace polymers derived from petroleum with superior biodegradable polymers (biopolymers). In this context, biopolymers are considered potential replacements for conventional plastic materials. However, some of their properties must be improved for better competitiveness, especially regarding their mechanical, thermal and barrier properties. Bio-nanocomposite technology using nanofillers has already been proven as an effective way to produce new materials with specific properties and high performances. With the emergence of nanostructured bio-composite materials, incorporating elongated rod-like cellulose nanocrystals (CNC) has attracted more and more attention in the field of nanotechnology. This study is aimed to develop bio-composite films of biopolymer matrices [Carboxymethyle cellulose (CMC), Starch (ST), Chitosan (CS) and Polyvinyl alcohol (PVA)] reinforced with cellulose nanocrystals (CNC) using the solution casting method. The CNC were extracted at a nanometric scale from lignocellulosic fibers via sulfuric acid hydrolysis and then characterized using X-ray diffraction (XRD), thermogravimetric analysis (TGA), confocal microscopy, infrared spectroscopy (IR), atomic force and transmission electron microscopies (AFM and TEM) techniques. The as extracted CNC were used as a reinforcing phase to produce a variety of bio-composite films at different CNC loading (0.5-10 wt %) with specific properties. The rheological properties of film-forming solutions (FFS) of bio-composites were studied, and their relation to the casting process was evaluated. Then, the structural, optical transparency, water vapor permeability, thermal stability and mechanical properties of all prepared bio-composite films were evaluated and studied in this report. The high performances of these bio-composite films are expected to have potential in biomaterials or packaging applications.

Keywords: biopolymer composites, cellulose nanocrystals, food packaging, lignocellulosic fibers

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Authors: Mohsen Adabi, Mahdi Adabi, Reza Saber

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The recent advancements in nanomaterials have provided a platform to develop efficient transduction matrices for sensors. Modified electrodes allow to electrochemists to enhance the property of electrode surface and provide desired properties such as improved sensing capabilities, higher electron transfer rate and prevention of undesirable reactions competing kinetically with desired electrode process. Nanostructured electrodes including arrays of carbon nanotubes have demonstrated great potential for the development of electrochemical sensors and biosensors. The aim of this work is to evaluate the concentration of multi-walled carbon nanotubes (MWCNTs) on the conductivity of gold electrode. For this work, raw MWCNTs was functionalized and shortened. Raw and shorten MWCNTs were characterized using transfer electron microscopy (TEM). Next, 0.5, 2 and 3.5 mg of Shortened and functionalized MWCNTs were dispersed in 2 mL Dimethyl formamide (DMF) and cysteamine modified gold electrodes were incubated in the different concentrations of MWCNTs for 8 hours. Then, the immobilization of MWCNTs on cysteamine modified gold electrode was characterized by scanning electron microscopy (SEM) and the effect of MWCNT concentrations on electron transfer of modified electrodes was investigated by cyclic voltammetry (CV). The results demonstrated that CV response of ferricyanide redox at modified gold electrodes increased as concentration of MWCNTs enhanced from 0.5 to 2 mg in 2 mL DMF. This increase can be attributed to the number of MWCNTs which enhance on the surface of cysteamine modified gold electrode as the MWCNTs concentration increased whereas CV response of ferricyanide redox at modified gold electrodes did not changed significantly as the MWCNTs concentration increased from 2 to 3.5 mg in 2 mL DMF. The reason may be that amine groups of cysteamine modified gold electrodes are limited to a given number which can interact with the given number of carboxylic groups of MWCNTs and CV response of ferricyanide redox at modified gold do not enhance after amine groups of cysteamine are saturated with carboxylic groups of MWCNTs.

Keywords: carbon nanotube, cysteamine, electrochemical sensor, gold electrode

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Authors: Joanna Cabaj, Sylwia Baluta, Karol Malecha, Kamila Drzozga

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Catecholamines are the principal neurotransmitters that mediate a variety of the central nervous system functions, such as motor control, cognition, emotion, memory processing, and endocrine modulation. Dysfunctions in catecholamine neurotransmission are induced in some neurologic and neuropsychiatric diseases. Changeable neurotransmitters level in biological fluids can be a marker of several neurological disorders. Because of its significance in analytical techniques and diagnostics, sensitive and selective detection of neurotransmitters is increasingly attracting a lot of attention in different areas of bio-analysis or biomedical research. Recently, fluorescent techniques for detection of catecholamines have attracted interests due to their reasonable cost, convenient control, as well as maneuverability in biological environments. Nevertheless, with the observed need for a sensitive and selective catecholamines sensor, the development of a convenient method for this neurotransmitter is still at its basic level. The manipulation of nanostructured materials in conjunction with biological molecules has led to the development of a new class of hybrid modified biosensors in which both enhancement of charge transport and biological activity preservation may be obtained. Immobilization of biomaterials on electrode surfaces is the crucial step in fabricating electrochemical as well as optical biosensors and bioelectronic devices. Continuing systematic investigation in the manufacturing of enzyme–conducting sensitive systems, here is presented a convenient fluorescence sensing strategy for catecholamines detection based on FRET (fluorescence resonance energy transfer) phenomena observed for, i.e., complexes of Fe²⁺ and epinephrine. The biosensor was constructed using low temperature co-fired ceramics technology (LTCC). This sensing system used the catalytical oxidation of catecholamines and quench of the strong luminescence of obtained complexes due to FRET. The detection process was based on the oxidation of substrate in the presence of the enzyme–laccase/tyrosinase.

Keywords: biosensor, conducting polymer, enzyme, FRET, LTCC

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Authors: Surya Prakash Gajagouni, Akram Alfantazi, Imad Barsoum

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Austenitic stainless steels are widely recognized for their exceptional corrosion resistance and mechanical properties, rendering them indispensable materials across various industries from construction to biomedical applications. However, in chloride and high temperature atmosphere it to further enhance their surface properties, anodization has emerged as a promising surface treatment technique. Anodization modifies the surface of stainless steels by creating a protective oxide layer, improving corrosion resistance and imparting additional functional characteristics. This paper explores the structural and corrosion characteristics of anodized austenitic stainless steels (AISI 304) using a two-step anodic technique. We utilized a perchloric acid-based electrolyte followed by an ammonium fluoride-based electrolyte. This sequential approach aimed to cultivate deeper and intricately self-ordered nanopore oxide arrays on a substrate made of 304 stainless steel. Electron Microscopic (SEM and TEM) images revealed nanoporous layered structures with increased length and crack development correlating with higher voltage and anodization time. Surface composition and chemical oxidation state of surface-treated SS were determined using X-ray photoelectron spectroscopy (XPS) techniques, revealing a surface layer rich in Ni and suppressed Cr, resulting in a thin film composed of Ni and Fe oxide compared to untreated SS. Electrochemical studies demonstrated enhanced corrosion resistance in a strong alkaline medium compared to untreated SS. Understanding the intricate relationship between the structural features of anodized stainless steels and their corrosion resistance is crucial for optimizing the performance of these materials in diverse applications. This study aims to contribute to the advancement of surface engineering strategies for enhancing the durability and functionality of austenitic stainless steels in aggressive environments.

Keywords: austenitic stainless steel, anodization, nanoporous oxides, marine corrosion

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Authors: Suveen Kumar

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Oral cancer (OC) is the sixth most death causing cancer in world which includes tumour of lips, floor of the mouth, tongue, palate, cheeks, sinuses, throat, etc. Conventionally, the techniques used for OC detection are toluidine blue staining, biopsy, liquid-based cytology, visual attachments, etc., however these are limited by their highly invasive nature, low sensitivity, time consumption, sophisticated instrument handling, sample processing and high cost. Therefore, we developed biosensing chips for non-invasive detection of OC via CYFRA-21-1 biomarker. CYFRA-21-1 (molecular weight: 40 kDa) is secreted in saliva of OC patients which is a non-invasive biological fluid with a cut-off value of 3.8 ng mL-1, above which the subjects will be suffering from oral cancer. Therefore, in first work, 3-aminopropyl triethoxy silane (APTES) functionalized zirconia (ZrO2) nanoparticles (APTES/nZrO2) were used to successfully detect CYFRA-21-1 in a linear detection range (LDR) of 2-16 ng mL-1 with sensitivity of 2.2 µA mL ng-1. Successively, APTES/nZrO2-RGO was employed to prevent agglomeration of ZrO2 by providing high surface area reduced graphene oxide (RGO) support and much wider LDR (2-22 ng mL-1) was obtained with remarkable limit of detection (LOD) as 0.12 ng mL-1. Further, APTES/nY2O3/ITO platform was used for oral cancer bioseneor development. The developed biosensor (BSA/anti-CYFRA-21-1/APTES/nY2O3/ITO) have wider LDR (0.01-50 ng mL-1) with remarkable limit of detection (LOD) as 0.01 ng mL-1. To improve the sensitivity of the biosensing platform, nanocomposite of yattria stabilized nanostructured zirconia-reduced graphene oxide (nYZR) based biosensor has been developed. The developed biosensing chip having ability to detect CYFRA-21-1 biomolecules in the range of 0.01-50 ng mL-1, LOD of 7.2 pg mL-1 with sensitivity of 200 µA mL ng-1. Further, the applicability of the fabricated biosensing chips were also checked through real sample (saliva) analysis of OC patients and the obtained results showed good correlation with the standard protein detection enzyme linked immunosorbent assay (ELISA) technique.

Keywords: non-invasive, oral cancer, nanomaterials, biosensor, biochip

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Authors: J. Tirano, H. Zea, C. Luhrs

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Photocatalysis has established as viable option in the development of processes for the treatment of pollutants and clean energy production. This option is based on the ability of semiconductors to generate an electron flow by means of the interaction with solar radiation. Owing to its electronic structure, TiO₂ is the most frequently used semiconductors in photocatalysis, although it has a high recombination of photogenerated charges and low solar energy absorption. An alternative to reduce these limitations is the use of nanostructured morphologies which can be produced during the synthesis of TiO₂ nanotubes (TNTs). Therefore, if possible to produce vertically oriented nanostructures it will be possible to generate a greater contact area with electrolyte and better charge transfer. At present, however, the development of these innovative structures still presents an important challenge for the development of competitive photoelectrochemical devices. This research focuses on established correlations between synthesis variables and 1D nanostructure morphology which has a direct effect on the photocatalytic performance. TNTs with controlled morphology were synthesized by two-step potentiostatic anodization of titanium foil. The anodization was carried out at room temperature in an electrolyte composed of ammonium fluoride, deionized water and ethylene glycol. Consequent thermal annealing of as-prepared TNTs was conducted in the air between 450 °C-550 °C. Morphology and crystalline phase of the TNTs were carried out by SEM, EDS and XRD analysis. As results, the synthesis conditions were established to produce nanostructures with specific morphological characteristics. Anatase was the predominant phase of TNTs after thermal treatment. Nanotubes with 10 μm in length, 40 nm in pore diameter and a surface-volume ratio of 50 are important in photoelectrochemical applications based on TiO₂ due to their 1D characteristics, high surface-volume ratio, reduced radial dimensions and high oxide/electrolyte interface. Finally, this knowledge can be used to improve the photocatalytic activity of TNTs by making additional surface modifications with dopants that improve their efficiency.

Keywords: electrochemical anodization, morphology, self-organized nanotubes, TiO₂ nanotubes

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Authors: Hanan. Al Chaghouri, Mohammad Azad Malik, P. John Thomas, Paul O’Brien

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The process of assembling metal nanoparticles at the interface of two liquids has received a great interest over the past few years due to a wide range of important applications and their unusual properties compared to bulk materials. We present a low cost, simple and cheap synthesis of metal nanoparticles, core/shell structures and semiconductors followed by assembly of these particles between immiscible liquids. The aim of this talk is divided to three parts: firstly, to describe the achievement of a closed loop recycling for producing cadmium sulphide as powders and/or nanostructured thin films for solar cells or other optoelectronic devices applications by using a different chain length of commercially available secondary amines of dithiocarbamato complexes. The approach can be extended to other metal sulphides such as those of Zn, Pb, Cu, or Fe and many transition metals and oxides. Secondly, to synthesis significantly cheaper magnetic particles suited for the mass market. Ni/NiO nanoparticles with ferromagnetic properties at room temperature were among the smallest and strongest magnets (5 nm) were made in solution. The applications of this work can be applied to produce viable storage devices and the other possibility is to disperse these nanocrystals in solution and use it to make ferro-fluids which have a number of mature applications. The third part is about preparing and assembling of submicron silver, cobalt and nickel particles by using polyol methods and liquid/liquid interface, respectively. Noble metal like gold, copper and silver are suitable for plasmonic thin film solar cells because of their low resistivity and strong interactions with visible light waves. Silver is the best choice for solar cell application since it has low absorption losses and high radiative efficiency compared to gold and copper. Assembled cobalt and nickel as films are promising for spintronic, magnetic and magneto-electronic and biomedics.

Keywords: assembling nanoparticles, liquid/liquid interface, thin film, core/shell, solar cells, recording media

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Authors: Neumoin Anton Ivanovich, Opra Denis Pavlovich

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Materials based on titanium oxide compounds are widely used in such areas as solar energy, photocatalysis, food industry and hygiene products, biomedical technologies, etc. Demand for them has also formed in the battery industry (an example of this is the commercialization of Li4Ti5O12), where much attention has recently been paid to the development of next-generation systems and technologies, such as sodium-ion batteries. This dictates the need to search for new materials with improved characteristics, as well as ways to obtain them that meet the requirements of scalability. One of the ways to solve these problems can be the creation of nanomaterials that often have a complex of physicochemical properties that radically differ from the characteristics of their counterparts in the micro- or macroscopic state. At the same time, it is important to control the texture (specific surface area, porosity) of such materials. In view of the above, among other methods, the hydrothermal technique seems to be suitable, allowing a wide range of control over the conditions of synthesis. In the present study, a method was developed for the preparation of mesoporous nanostructured sodium trititanate (Na2Ti3O7) with a hierarchical architecture. The materials were synthesized by hydrothermal processing and exhibit a complex hierarchically organized two-layer architecture. At the first level of the hierarchy, materials are represented by particles having a roughness surface, and at the second level, by one-dimensional nanotubes. The products were found to have high specific surface area and porosity with a narrow pore size distribution (about 6 nm). As it is known, the specific surface area and porosity are important characteristics of functional materials, which largely determine the possibilities and directions of their practical application. Electrochemical impedance spectroscopy data show that the resulting sodium trititanate has a sufficiently high electrical conductivity. As expected, the synthesized complexly organized nanoarchitecture based on sodium trititanate with a porous structure can be practically in demand, for example, in the field of new generation electrochemical storage and energy conversion devices.

Keywords: sodium trititanate, hierarchical materials, mesoporosity, nanotubes, hydrothermal synthesis

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Authors: Mariana-Dana Damaceanu

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Electrochemical oxidation is one of the most convenient ways to obtain conjugated polymer films as polypyrrole, polyaniline, polythiophene or polycarbazole. The research in the field has been mainly directed to the study of electrical conduction properties of the materials obtained by electropolymerization, often the main reason being their use as electroconducting electrodes, and very little attention has been paid to the morphological and optical quality of the films electrodeposited on flat surfaces. Electropolymerization of the monomer solution was scarcely used in the past to manufacture polymer-based light-emitting diodes (PLED), most probably due to the difficulty of obtaining defectless polymer films with good mechanical and optical properties, or conductive polymers with well controlled molecular weights. Here we report our attempts in using electrochemical deposition as appropriate method for preparing ultrathin films of fluorene-based polymers for PLED applications. The properties of these films were evaluated in terms of structural morphology, optical properties, and electrochemical conduction. Thus, electropolymerization of 4,4'-(9-fluorenylidene)-dianiline was performed in dichloromethane solution, at a concentration of 10-2 M, using 0.1 M tetrabutylammonium tetrafluoroborate as electrolyte salt. The potential was scanned between 0 and 1.3 V on the one hand, and 0 - 2 V on the other hand, when polymer films with different structures and properties were obtained. Indium tin oxide-coated glass substrate of different size was used as working electrode, platinum wire as counter electrode and calomel electrode as reference. For each potential range 100 cycles were recorded at a scan rate of 100 mV/s. The film obtained in the potential range from 0 to 1.3 V, namely poly(FDA-NH), is visible to the naked eye, being light brown, transparent and fluorescent, and displays an amorphous morphology. Instead, the electrogrowth poly(FDA) film in the potential range of 0 - 2 V is yellowish-brown and opaque, presenting a self-assembled structure in aggregates of irregular shape and size. The polymers structure was identified by FTIR spectroscopy, which shows the presence of broad bands specific to a polymer, the band centered at approx. 3443 cm-1 being ascribed to the secondary amine. The two polymer films display two absorption maxima, at 434-436 nm assigned to π-π* transitions of polymers, and another at 832 and 880 nm assigned to polaron transitions. The fluorescence spectra indicated the presence of emission bands in the blue domain, with two peaks at 422 and 488 nm for poly (FDA-NH), and four narrow peaks at 422, 447, 460 and 484 nm for poly(FDA), peaks originating from fluorene-containing segments of varying degrees of conjugation. Poly(FDA-NH) exhibited two oxidation peaks in the anodic region and the HOMO energy value of 5.41 eV, whereas poly(FDA) showed only one oxidation peak and the HOMO level localized at 5.29 eV. The electrochemical data are discussed in close correlation with the proposed chemical structure of the electrogrowth films. Further research will be carried out to study their use and performance in light-emitting devices.

Keywords: electrogrowth polymer films, fluorene, morphology, optical properties

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Authors: L. Mentar, O. Baka, A. Azizi

Abstract:

Zinc oxide as a wide band semiconductor materials, especially nanostructured materials, have potential applications in large-area such as electronics, sensors, photovoltaic cells, photonics, optical devices and optoelectronics due to their unique electrical and optical properties and surface properties. The feasibility of ZnO for these applications is due to the successful synthesis of diverse ZnO nanostructures, including nanorings, nanobows, nanohelixes, nanosprings, nanobelts, nanotubes, nanopropellers, nanodisks, and nanocombs, by different method. Among various synthesis methods, electrochemical deposition represents a simple and inexpensive solution based method for synthesis of semiconductor nanostructures. In this study, the electrodeposition method was used to produce zinc oxide (ZnO) nanostructures on fluorine-doped tin oxide (FTO)-coated conducting glass substrate as TCO from chloride bath. We present a systematic study on the effects of the concentration of chloride anion on the properties of ZnO. The influence of KCl concentrations on the electrodeposition process, morphological, structural and optical properties of ZnO nanostructures was examined. In this research electrochemical deposition of ZnO nanostructures is investigated using conventional electrochemical measurements (cyclic voltammetry and Mott-Schottky), scanning electron microscopy (SEM), and X-ray diffraction (XRD) techniques. The potentials of electrodeposition of ZnO were determined using the cyclic voltammetry. From the Mott-Schottky measurements, the flat-band potential and the donor density for the ZnO nanostructure are determined. SEM images shows different size and morphology of the nanostructures and depends greatly on the KCl concentrations. The morphology of ZnO nanostructures is determined by the corporated action between [Zn(NO3)2] and [Cl-].Very netted hexagonal grains are observed for the nanostructures deposited at 0.1M of KCl. XRD studies revealed that the all deposited films were polycrystalline in nature with wurtzite phase. The electrodeposited thin films are found to have preferred oriented along (002) plane of the wurtzite structure of ZnO with c-axis normal to the substrate surface for sample at different concentrations of KCl. UV-Visible spectra showed a significant optical transmission (~80%), which decreased with low Cl-1 concentrations. The energy band gap values have been estimated to be between 3.52 and 3.80 eV.

Keywords: electrodeposition, ZnO, chloride ions, Mott-Schottky, SEM, XRD

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Authors: Hanan. Al Chaghouri, Mohammad Azad Malik, P. John Thomas, Paul O’Brien

Abstract:

The process of assembling metal nanoparticles at the interface of two liquids has received a great deal of attention over the past few years due to a wide range of important applications and their unusual properties as compared to bulk materials. We present a low cost, simple and cheap synthesis of metal nanoparticles, core/shell structures and semiconductors followed by assembly of these particles between immiscible liquids. The aim of this talk is divided to three parts: Firstly, to describe the achievement of a closed loop recycling for producing cadmium sulfide as powders and/or nanostructured thin films for solar cells or other optoelectronic devices applications by using a different chain length of commercially available secondary amines of dithiocarbamato complexes. The approach can be extended to other metal sulfides such as those of Zn, Pb, Cu, or Fe and many transition metals and oxides. Secondly, to synthesis significantly cheaper magnetic particles suited for the mass market. Ni/NiO nanoparticles with ferromagnetic properties at room temperature were among the smallest and strongest magnets (5 nm) were made in solution. The applications of this work can be to produce viable storage devices and the other possibility is to disperse these nanocrystals in solution and use it to make ferrofluids which have a number of mature applications. The third part is about preparing and assembling of submicron silver, cobalt and nickel particles by using polyol methods and liquid/liquid interface, respectively. Coinage metals like gold, copper and silver are suitable for plasmonic thin film solar cells because of their low resistivity and strong interactions with visible light waves. Silver is the best choice for solar cell application since it has low absorption losses and high radiative efficiency compared to gold and copper. Assembled cobalt and nickel as films are promising for spintronic, magnetic and magneto-electronic and biomedics.

Keywords: metal nanoparticles, core/shell structures and semiconductors, ferromagnetic properties, closed loop recycling, liquid/liquid interface

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Authors: Sourav Biswas, Goutam Prasanna Kar, Suryasarathi Bose

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In order to obtain better materials, control in the precise location of nanoparticles is indispensable. It was shown here that ordered arrangement of nanoparticles, possessing different characteristics (electrical/magnetic dipoles), in the blend structure can result in excellent microwave absorption. This is manifested from a high reflection loss of ca. -67 dB for the best blend structure designed here. To attenuate electromagnetic radiations, the key parameters i.e. high electrical conductivity and large dielectric/magnetic loss are targeted here using a conducting inclusion [multiwall carbon nanotubes, MWNTs]; ferroelectric nanostructured material with associated relaxations in the GHz frequency [barium titanate, BT]; and a loss ferromagnetic nanoparticles [nickel ferrite, NF]. In this study, bi-continuous structures were designed using 50/50 (by wt) blends of polycarbonate (PC) and polyvinylidene fluoride (PVDF). The MWNTs was modified using an electron acceptor molecule; a derivative of perylenediimide, which facilitates π-π stacking with the nanotubes and stimulates efficient charge transport in the blends. The nanoscopic materials have specific affinity towards the PVDF phase. Hence, by introducing surface-active groups, ordered arrangement can be tailored. To accomplish this, both BT and NF was first hydroxylated followed by introducing amine-terminal groups on the surface. The latter facilitated in nucleophilic substitution reaction with PC and resulted in their precise location. In this study, we have shown for the first time that by compartmentalized approach, superior EM attenuation can be achieved. For instance, when the nanoparticles were localized exclusively in the PVDF phase or in both the phases, the minimum reflection loss was ca. -18 dB (for MWNT/BT mixture) and -29 dB (for MWNT/NF mixture), and the shielding was primarily through reflection. Interestingly, by adopting the compartmentalized approach where in, the lossy materials were in the PC phase and the conducting inclusion (MWNT) in PVDF, an outstanding reflection loss of ca. -57 dB (for BT and MWNT combination) and -67 dB (for NF and MWNT combination) was noted and the shielding was primarily through absorption. Thus, the approach demonstrates that nanoscopic structuring in the blends can be achieved under macroscopic processing conditions and this strategy can further be explored to design microwave absorbers.

Keywords: barium titanate, EMI shielding, MWNTs, nickel ferrite

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Authors: J. Tirano, H. Zea, C. Luhrs

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It is well known that titanium dioxide is a semiconductor with several applications in photocatalytic process. Its band gap makes it very interesting in the photoelectrodes manufacturing used in photoelectrochemical cells for hydrogen production, a clean and environmentally friendly fuel. The synthesis of 1D titanium dioxide nanostructures, such as nanotubes, makes possible to produce more efficient photoelectrodes for solar energy to hydrogen conversion. In essence, this is because it increases the charge transport rate, decreasing recombination options. However, its principal constraint is to be mainly sensitive to UV range, which represents a very low percentage of solar radiation that reaches earth's surface. One of the alternatives to modifying the TiO2’s band gap and improving its photoactivity under visible light irradiation is to dope the nanotubes with transition metals. This option requires fabricating efficient nanostructured photoelectrodes with controlled morphology and specific properties able to offer a suitable surface area for metallic doping. Hence, currently one of the central challenges in photoelectrochemical cells is the construction of nanomaterials with a proper band position for driving the reaction while absorbing energy over the VIS spectrum. This research focuses on the synthesis and characterization of Nidoped TiO2 nanotubes for improving its photocatalytic activity in solar energy conversion applications. Initially, titanium dioxide nanotubes (TNTs) with controlled morphology were synthesized by two-step potentiostatic anodization of titanium foil. The anodization was carried out at room temperature in an electrolyte composed of ammonium fluoride, deionized water and ethylene glycol. Consequent thermal annealing of as-prepared TNTs was conducted in the air between 450 °C - 550 °C. Afterwards, the nanotubes were superficially modified by nickel deposition. Morphology and crystalline phase of the samples were carried out by SEM, EDS and XRD analysis before and after nickel deposition. Determining the photoelectrochemical performance of photoelectrodes is based on typical electrochemical characterization techniques. Also, the morphological characterization associated electrochemical behavior analysis were discussed to establish the effect of nickel nanoparticles modification on the TiO2 nanotubes. The methodology proposed in this research allows using other transition metal for nanotube surface modification.

Keywords: dimensionally stable electrode, nickel nanoparticles, photo-electrode, TiO₂ nanotubes

Procedia PDF Downloads 151

Authors: Mohamed S. Selim, Nesreen A. Fatthallah, Shimaa A. Higazy, Hekmat R. Madian, Sherif A. El-Safty, Mohamed A. Shenashen

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After the 2003 prohibition on employing TBT-based antifouling coatings, polysiloxane antifouling nano-coatings have gained in popularity as environmentally friendly and cost-effective replacements. A series of non-toxic polydimethylsiloxane nanocomposites filled with nanosheets of graphene oxide (GO) decorated with magnetite nanospheres (GO-Fe₃O₄ nanospheres) were developed and cured via a catalytic hydrosilation method. Various GO-Fe₃O₄ hybrid concentrations were mixed with the silicone resin via solution casting technique to evaluate the structure–property connection. To generate GO nanosheets, a modified Hummers method was applied. A simple co-precipitation method was used to make spherical magnetite particles under inert nitrogen. Hybrid GO-Fe₃O₄ composite fillers were developed by a simple ultrasonication method. Superhydrophobic PDMS/GO-Fe₃O₄ nanocomposite surface with a micro/nano-roughness, reduced surface-free energy (SFE), high fouling release (FR) efficiency was achieved. The physical, mechanical, and anticorrosive features of the virgin and GO-Fe₃O₄ filled nanocomposites were investigated. The synergistic effects of GO-Fe₃O4 hybrid's well-dispersion on the water-repellency and surface topological roughness of the PDMS/GO-Fe₃O₄ nanopaints were extensively studied. The addition of the GO-Fe₃O₄ hybrid fillers till 1 wt.% could increase the coating's water contact angle (158°±2°), minimize its SFE to 12.06 mN/m, develop outstanding micro/nano-roughness, and improve its bulk mechanical and anticorrosion properties. Several microorganisms were employed for examining the fouling-resistance of the coated specimens for 1 month. Silicone coatings filled with 1 wt.% GO-Fe₃O₄ nanofiller showed the least biodegradability% among all the tested microorganisms. Whereas GO-Fe₃O4 with 5 wt.% nanofiller possessed the highest biodegradability% potency by all the microorganisms. We successfully developed non-toxic and low cost nanostructured FR composite coating with high antifouling-resistance, reproducible superhydrophobic character, and enhanced service-time for maritime navigation.

Keywords: silicone antifouling, environmentally friendly, nanocomposites, nanofillers, fouling repellency, hydrophobicity

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Authors: Suzanne Giasson, Alberto Guerron

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Stimuli-responsive polymer coatings can be used as functional elements in nanotechnologies, such as valves in microfluidic devices, as membranes in biomedical engineering, as substrates for the culture of biological tissues or in developing nanomaterials for targeted therapies in different diseases. However, such coatings usually suffer from major shortcomings, such as a lack of selectivity and poor environmental stability. The study will present multi-responsive hierarchical and hybrid polymer-based coatings aiming to overcome some of these limitations. Hierarchical polymer coatings, consisting of two-dimensional arrays of thermo-responsive cationic PNIPAM-based microgels and surface-functionalized with non-responsive or pH-responsive polymers, were covalently grafted to substrates to tune the surface chemistry and the elasticity of the surface independently using different stimuli. The characteristic dimensions (i.e., layer thickness) and surface properties (i.e., adhesion, friction) of the microgel coatings were assessed using the Surface Forces Apparatus. The ability to independently control the swelling and surface properties using temperature and pH as triggers were investigated for microgels in aqueous suspension and microgels immobilized on substrates. Polymer chain grafting did not impede the ability of cationic PNIPAM microgels to undergo a volume phase transition above the VPTT, either in suspension or immobilized on a substrate. Due to the presence of amino groups throughout the entirety of the microgel polymer network, the swelling behavior was also pH dependent. However, the thermo-responsive swelling was more significant than the pH-triggered one. The microgels functionalized with PEG exhibited the most promising behavior. Indeed, the thermo-triggered swelling of microgel-co-PEG did not give rise to changes in the microgel surface properties (i.e., surface potential and adhesion) within a wide range of pH values. It was possible for the immobilized microgel-co-PEG to undergo a volume transition (swelling/shrinking) with no change in adhesion, suggesting that the surface of the thermal-responsive microgels remains rather hydrophilic above the VPTT. This work confirms the possibility of tuning the swelling behavior of microgels without changing the adhesive properties. Responsive surfaces whose swelling properties can be reversibly and externally altered over space and time regardless of the surface chemistry are very innovative and will enable revolutionary advances in technologies, particularly in biomedical surface engineering and microfluidics, where advanced assembly of functional components is increasingly required.

Keywords: responsive materials, polymers, surfaces, cell culture

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Authors: Esmeralda Chávez Vargas, M. de la L. Olvera, A. Maldonado

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The doping it is believed as follows, at high concentration fluorine in ZnO: F films is incorporated to the lattice by substitution of O-2 ions by F-1 ions; at middle fluorine concentrations, F ions may form interstitials, whereas for low concentrations it is increased the carriers and mobility could be explained by the surface passivation effect of fluorine. ZnO:F thin films were deposited on sodocalcic glass substratesat 425 °C , 450°C, 475 during 8, 12, 15 min from a 0.2 M solution. Doping concentration in the starting solutions was varied, namely, [F]/[F+Zn] = 0, 5, 15, 30, 45, 60, and 90 at. %; solvent composition was varied as well, 100:100; 50:50; 100:50(acetic acid: water: methanol ratios, in volume). In this work it is reported the characterization results of fluorine doped zinc oxide (ZnO:F) thin films deposited by the ultrasonic spray pyrolysis technique, using zinc acetate and ammonium fluorine as Zn an F precursors, respectively. The effect of varying the fluorine concentration in the starting solutions, the solvent composition, and the ageing time of the starting solutions, on the electrical resistivity, optical transmittance, structure and surface morphology was analyzed. In order to have a quantitative evaluation of the ZnO:F thin films for its application as transparent electrodes, the Figure of Merit was estimated from the Haacke´s formula. After a thoroughly study, it can be found that optimal conditions for the deposition of transparent and conductive ZnO:F thin films on sodocalcic substrates, were as follows; substrate temperature: solution molar concentration 0.2, doping concentration in the starting solution of [F]/[Zn]= 60 at. %, (water content)/(acetic acid) in starting solution: [H2O/ CH3OH]= 50:50, substrate temperature: 450 °C. The effects of aging of the starting solution has also been analyzed thoroughly and it has been found a dramatic effect on the electric resistivity of the material, aged by 40 days, show an electrical resitivity as low as 120 Ω/□, with a transmittance around 80% in the visible range. X-ray diffraction spectra show a polycrystalline of ZnO (wurtzite structure) where the amount of fluorine doping affects to preferential orientation (002 plane). Therefore, F introduction in lattice is by the substitution of O-2 ions by F-1 ions. The results show that ZnO:F thin films are potentially adequate for application as transparent conductive oxide in thin film solar cells.

Keywords: TCOs, transparent electrodes, ultrasonic spray pyrolysis, zinc oxide, ZnO:F

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Authors: Sarathlal Koyiloth Vayalil, Stephan V. Roth, Gonzalo Santoro, Peng Zhang, Matthias Schwartzkopf, Bjoern Beyersdorff

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Nanostructured magnetic thin films have gained significant relevance due to its applications in magnetic storage and recording media. Self-organized arrays of nanoparticles and nanowires can be produced by depositing metal thin films on nano-rippled substrates. The substrate topography strongly affects the film growth giving rise to anisotropic properties (optical, magnetic, electronic transport). Ion-beam erosion (IBE) method can provide large-area patterned substrates with the valuable possibility to widely modify pattern length scale by simply acting on ion beam parameters (i.e. energy, ions, geometry, etc.). In this work, investigation of the growth mechanism of Permalloy thin films on such nano-rippled Si (100) substrates using in situ grazing incidence small angle x-ray scattering measurements (GISAXS) have been done. In situ GISAXS measurements during the deposition of thin films have been carried out at the P03/MiNaXS beam line of PETRA III storage ring of DESY, Hamburg. Nanorippled Si substrates prepared by low energy ion beam sputtering with an average wavelength of 33 nm and 1 nm have been used as templates. It has been found that the film replicates the morphology up to larger thickness regimes and also the growth is highly anisotropic along and normal to the ripple wave vectors. Various growth regimes have been observed. Further, magnetic measurements have been done using magneto-optical Kerr effect by rotating the sample in the azimuthal direction. Strong uniaxial magnetic anisotropy with its easy axis in a direction normal to the ripple wave vector has been observed. The strength of the magnetic anisotropy is found to be decreasing with increasing thin film thickness values. The mechanism of the observed strong uniaxial magnetic anisotropy and its depends on the thickness of the film has been explained by correlating it with the GISAXS results. In conclusion, we have done a detailed growth analysis of Permalloy thin films deposited on nanorippled Si templates and tried to explain the correlation between structure, morphology to the observed magnetic properties.

Keywords: grazing incidence small angle x-ray scattering, magnetic thin films, magnetic anisotropy, nanoripples

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Authors: A. Rezaei, M. Huisman, W. Van Paepegem

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Atomic interactions in molecular systems are mainly studied by particle mechanics. Nevertheless, researches have also put on considerable effort to simulate them using continuum methods. In early 2000, simple equivalent finite element models have been developed to study the mechanical properties of carbon nanotubes and graphene in composite materials. Afterward, many researchers have employed similar structural simulation approaches to obtain mechanical properties of nanostructured materials, to simplify interface behavior of fiber-reinforced composites, and to simulate defects in carbon nanotubes or graphene sheets, etc. These structural approaches, however, are limited to small deformations due to complicated local rotational coordinates. This article proposes a method for the finite element simulation of molecular mechanics. For ease in addressing the approach, here it is called Structural Finite Element Molecular Modeling (SFEMM). SFEMM method improves the available structural approaches for large deformations, without using any rotational degrees of freedom. Moreover, the method simulates molecular conformation, which is a big advantage over the previous approaches. Technically, this method uses nonlinear multipoint constraints to simulate kinematics of the atomic multibody interactions. Only truss elements are employed, and the bond potentials are implemented through constitutive material models. Because the equilibrium bond- length, bond angles, and bond-torsion potential energies are intrinsic material parameters, the model is independent of initial strains or stresses. In this paper, the SFEMM method has been implemented in ABAQUS finite element software. The constraints and material behaviors are modeled through two Fortran subroutines. The method is verified for the bond-stretch, bond-angle and bond-torsion of carbon atoms. Furthermore, the capability of the method in the conformation simulation of molecular structures is demonstrated via a case study of a graphene sheet. Briefly, SFEMM builds up a framework that offers more flexible features over the conventional molecular finite element models, serving the structural relaxation modeling and large deformations without incorporating local rotational degrees of freedom. Potentially, the method is a big step towards comprehensive molecular modeling with finite element technique, and thereby concurrently coupling an atomistic domain to a solid continuum domain within a single finite element platform.

Keywords: finite element, large deformation, molecular mechanics, structural method

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Authors: Fatima Zahra Mahjoubi, Abderrahim Khalidi, Mohamed Abdennouri, Omar Cherkaoui, Noureddine Barka

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Industrial effluents are one of the major causes of environmental pollution, especially effluents discharged from various dyestuff manufactures, plastic, and paper making industries. These effluents can give rise to certain hazards and environmental problems for their highly colored suspended organic solid. Dye effluents are not only aesthetic pollutants, but coloration of water by the dyes may affect photochemical activities in aquatic systems by reducing light penetration. It has been also reported that several commonly used dyes are carcinogenic and mutagenic for aquatic organisms. Therefore, removing dyes from effluents is of significant importance. Many adsorbent materials have been prepared in the removal of dyes from wastewater, including anionic clay or layered double hydroxyde. The zinc/aluminium (Zn-AlNO₃), magnesium/aluminium (Mg-AlNO₃) and nickel/aluminium (Ni-AlNO₃) layered double hydroxides (LDHs) were successfully synthesized via coprecipitation method. Samples were characterized by XRD, FTIR, TGA/DTA, TEM and pHPZC analysis. XRD patterns showed a basal spacing increase in the order of Zn-AlNO₃ (8.85Å)> Mg-AlNO₃ (7.95Å)> Ni-AlNO₃ (7.82Å). FTIR spectrum confirmed the presence of nitrate anions in the LDHs interlayer. The TEM images indicated that the Zn-AlNO3 presents circular to shaped particles with an average particle size of approximately 30 to 40 nm. Small plates assigned to sheets with hexagonal form were observed in the case of Mg-AlNO₃. Ni-AlNO₃ display nanostructured sphere in diameter between 5 and 10 nm. The LDHs were used as adsorbents for the removal of methyl orange (MO), as a model dye and for the treatment of an effluent generated by a textile factory. Adsorption experiments for MO were carried out as function of solution pH, contact time and initial dye concentration. Maximum adsorption was occurred at acidic solution pH. Kinetic data were tested using pseudo-first-order and pseudo-second-order kinetic models. The best fit was obtained with the pseudo-second-order kinetic model. Equilibrium data were correlated to Langmuir and Freundlich isotherm models. The best conditions for color and COD removal from textile effluent sample were obtained at lower values of pH. Total color removal was obtained with Mg-AlNO₃ and Ni-AlNO₃ LDHs. Reduction of COD to limits authorized by Moroccan standards was obtained with 0.5g/l LDHs dose.

Keywords: chemical oxygen demand, color removal, layered double hydroxides, textile wastewater treatment

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Authors: Karolina Ordon, Sandrine Coste, Malgorzata Makowska-Janusik, Abdelhadi Kassiba

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Photocatalytic processes play key role in the production of a new source of energy (as hydrogen), design of self-cleaning surfaces or for the environment preservation. The most challenging task deals with the purification of water distinguished by high efficiency. In the mentioned process, organic pollutants in solutions are decomposed to the simple, non-toxic compounds as H2O and CO2. The most known photocatalytic materials are ZnO, CdS and TiO2 semiconductors with a particular involvement of TiO2 as an efficient photocatalysts even with a high band gap equal to 3.2 eV which exploit only UV radiation from solar emitted spectrum. However, promising material with visible light induced photoactivity was searched through the monoclinic polytype of BiVO4 which has energy gap about 2.4 eV. As required in heterogeneous photocatalysis, the high contact surface is required. Also, BiVO4 as photocatalyst can be optimized by increasing its surface area by achieving the mesoporous structure synthesize. The main goal of the present work consists in the synthesis and characterization of BiVO4 mesoporous thin film. The synthesis method based on sol-gel was carried out using a standard surfactants such as P123 and F127. The thin film was deposited by spin and dip coating method. Then, the structural analysis of the obtained material was performed thanks to X-ray diffraction (XRD) and Raman spectroscopy. The surface of resulting structure was investigated using a scanning electron microscopy (SEM). The computer simulations based on modeling the optical and electronic properties of bulk BiVO4 by using DFT (density functional theory) methodology were carried out. The semiempirical parameterized method PM6 was used to compute the physical properties of BiVO4 nanostructures. The Raman and IR absorption spectra were also measured for synthesized mesoporous material, and the results were compared with the theoretical predictions. The simulations of nanostructured BiVO4 have pointed out the occurrence of quantum confinement for nanosized clusters leading to widening of the band gap. This result overcame the relevance of nanosized objects to harvest wide part of the solar spectrum. Also, a balance was searched experimentally through the mesoporous nature of the films devoted to enhancing the contact surface as required for heterogeneous catalysis without to lower the nanocrystallite size under some critical sizes inducing an increased band gap. The present contribution will discuss the relevant features of the mesoporous films with respect to their photocatalytic responses.

Keywords: bismuth vanadate, photocatalysis, thin film, quantum-chemical calculations

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Authors: Maksudur Rahman Khan, Kar Min Chan, Huei Ruey Ong, Chin Kui Cheng, Wasikur Rahman

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Microbial fuel cells (MFCs) represent a promising technology for simultaneous bioelectricity generation and wastewater treatment. Catalysts are significant portions of the cost of microbial fuel cell cathodes. Many materials have been tested as aqueous cathodes, but air-cathodes are needed to avoid energy demands for water aeration. The sluggish oxygen reduction reaction (ORR) rate at air cathode necessitates efficient electrocatalyst such as carbon supported platinum catalyst (Pt/C) which is very costly. Manganese oxide (MnO2) was a representative metal oxide which has been studied as a promising alternative electrocatalyst for ORR and has been tested in air-cathode MFCs. However, the single MnO2 has poor electric conductivity and low stability. In the present work, the MnO2 catalyst has been modified by doping Pt nanoparticle. The goal of the work was to improve the performance of the MFC with minimum Pt loading. MnO2 and Pt nanoparticles were prepared by hydrothermal and sol-gel methods, respectively. Wet impregnation method was used to synthesize Pt/MnO2 catalyst. The catalysts were further used as cathode catalysts in air-cathode cubic MFCs, in which anaerobic sludge was inoculated as biocatalysts and palm oil mill effluent (POME) was used as the substrate in the anode chamber. The as-prepared Pt/MnO2 was characterized comprehensively through field emission scanning electron microscope (FESEM), X-Ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and cyclic voltammetry (CV) where its surface morphology, crystallinity, oxidation state and electrochemical activity were examined, respectively. XPS revealed Mn (IV) oxidation state and Pt (0) nanoparticle metal, indicating the presence of MnO2 and Pt. Morphology of Pt/MnO2 observed from FESEM shows that the doping of Pt did not cause change in needle-like shape of MnO2 which provides large contacting surface area. The electrochemical active area of the Pt/MnO2 catalysts has been increased from 276 to 617 m2/g with the increase in Pt loading from 0.2 to 0.8 wt%. The CV results in O2 saturated neutral Na2SO4 solution showed that MnO2 and Pt/MnO2 catalysts could catalyze ORR with different catalytic activities. MFC with Pt/MnO2 (0.4 wt% Pt) as air cathode catalyst generates a maximum power density of 165 mW/m3, which is higher than that of MFC with MnO2 catalyst (95 mW/m3). The open circuit voltage (OCV) of the MFC operated with MnO2 cathode gradually decreased during 14 days of operation, whereas the MFC with Pt/MnO2 cathode remained almost constant throughout the operation suggesting the higher stability of the Pt/MnO2 catalyst. Therefore, Pt/MnO2 with 0.4 wt% Pt successfully demonstrated as an efficient and low cost electrocatalyst for ORR in air cathode MFC with higher electrochemical activity, stability and hence enhanced performance.

Keywords: microbial fuel cell, oxygen reduction reaction, Pt/MnO2, palm oil mill effluent, polarization curve

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Authors: Ingrid Snustad, Asmund Ervik, Anders Austegard, Amy Brunsvold, Jianying He, Zhiliang Zhang

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CO₂ capture, transport and storage (CCS) is essential to mitigate global anthropogenic CO₂ emissions. To make CCS a widely implemented technology in, e.g. the power sector, the reduction of costs is crucial. For a large cost reduction, every part of the CCS chain must contribute. By increasing the heat transfer efficiency during liquefaction of CO₂, which is a necessary step, e.g. ship transportation, the costs associated with the process are reduced. Heat transfer rates during dropwise condensation are up to one order of magnitude higher than during filmwise condensation. Dropwise condensation usually occurs on a non-wetting surface (Superlyophobic surface). The vapour condenses in discrete droplets, and the non-wetting nature of the surface reduces the adhesion forces and results in shedding of condensed droplets. This, again, results in fresh nucleation sites for further droplet condensation, effectively increasing the liquefaction efficiency. In addition, the droplets in themselves have a smaller heat transfer resistance than a liquid film, resulting in increased heat transfer rates from vapour to solid. Surface tension is a crucial parameter for dropwise condensation, due to its impact on the solid-liquid contact angle. A low surface tension usually results in a low contact angle, and again to spreading of the condensed liquid on the surface. CO₂ has very low surface tension compared to water. However, at relevant temperatures and pressures for CO₂ condensation, the surface tension is comparable to organic compounds such as pentane, a dropwise condensation of CO₂ is a completely new field of research. Therefore, knowledge of several important parameters such as contact angle and drop size distribution must be gained in order to understand the nature of the condensation. A new setup has been built to measure these relevant parameters. The main parts of the experimental setup is a pressure chamber in which the condensation occurs, and a high- speed camera. The process of CO₂ condensation is visually monitored, and one can determine the contact angle, contact angle hysteresis and hence, the surface adhesion of the liquid. CO₂ condensation on different surfaces can be analysed, e.g. copper, aluminium and stainless steel. The experimental setup is built for accurate measurements of the temperature difference between the surface and the condensing vapour and accurate pressure measurements in the vapour. The temperature will be measured directly underneath the condensing surface. The next step of the project will be to fabricate nanostructured surfaces for inducing superlyophobicity. Roughness is a key feature to achieve contact angles above 150° (limit for superlyophobicity) and controlled, and periodical roughness on the nanoscale is beneficial. Surfaces that are non- wetting towards organic non-polar liquids are candidates surface structures for dropwise condensation of CO₂.

Keywords: CCS, dropwise condensation, low surface tension liquid, superlyophobic surfaces

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Authors: Irina Veselova, Maria Makedonskaya, Olga Eremina, Alexandr Sidorov, Eugene Goodilin, Tatyana Shekhovtsova

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Such catecholamines as dopamine, norepinephrine, and epinephrine are the principal neurotransmitters in the sympathetic nervous system. Catecholamines and their metabolites are considered to be important markers of socially significant diseases such as atherosclerosis, diabetes, coronary heart disease, carcinogenesis, Alzheimer's and Parkinson's diseases. Currently, neurotransmitters can be studied via electrochemical and chromatographic techniques that allow their characterizing and quantification, although these techniques can only provide crude spatial information. Besides, the difficulty of catecholamine determination in biological materials is associated with their low normal concentrations (~ 1 nM) in biomaterials, which may become even one more order lower because of some disorders. In addition, in blood they are rapidly oxidized by monoaminooxidases from thrombocytes and, for this reason, the determination of neurotransmitter metabolism indicators in an organism should be very rapid (15—30 min), especially in critical states. Unfortunately, modern instrumental analysis does not offer a complex solution of this problem: despite its high sensitivity and selectivity, HPLC-MS cannot provide sufficiently rapid analysis, while enzymatic biosensors and immunoassays for the determination of the considered analytes lack sufficient sensitivity and reproducibility. Fluorescent and SERS-sensors remain a compelling technology for approaching the general problem of selective neurotransmitter detection. In recent years, a number of catecholamine sensors have been reported including RNA aptamers, fluorescent ribonucleopeptide (RNP) complexes, and boronic acid based synthetic receptors and the sensor operated in a turn-off mode. In this work we present the fluorescent and SERS turn-on sensor systems based on the bio- or chemorecognizing nanostructured films {chitosan/collagen-Tb/Eu/Cu-nanoparticles-indicator reagents} that provide the selective recognition, visualization, and sensing of the above mentioned catecholamines on the level of nanomolar concentrations in biomaterials (cell cultures, tissue etc.). We have (1) developed optically transparent porous films and gels of chitosan/collagen; (2) ensured functionalization of the surface by molecules-'recognizers' (by impregnation and immobilization of components of the indicator systems: biorecognizing and auxiliary reagents); (3) performed computer simulation for theoretical prediction and interpretation of some properties of the developed materials and obtained analytical signals in biomaterials. We are grateful for the financial support of this research from Russian Foundation for Basic Research (grants no. 15-03-05064 a, and 15-29-01330 ofi_m).

Keywords: biomaterials, fluorescent and SERS-recognition, neurotransmitters, solid-phase turn-on sensor system

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Authors: Peter Kus, Anna Ostroverkh, Yurii Yakovlev, Yevheniia Lobko, Roman Fiala, Ivan Khalakhan, Vladimir Matolin

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Hydrogen economy is a concept of low-emission society which harvests most of its energy from renewable sources (e.g., wind and solar) and in case of overproduction, electrochemically turns the excess amount into hydrogen, which serves as an energy carrier. Proton exchange membrane water electrolyzers (PEMWE) are the backbone of this concept. By fast-response electricity to hydrogen conversion, the PEMWEs will not only stabilize the electrical grid but also provide high-purity hydrogen for variety of fuel cell powered devices, ranging from consumer electronics to vehicles. Wider commercialization of PEMWE technology is however hindered by high prices of noble metals which are necessary for catalyzing the redox reactions within the cell. Namely, platinum for hydrogen evolution reaction (HER), running on cathode, and iridium for oxygen evolution reaction (OER) on anode. Possible way of how to lower the loading of Pt and Ir is by using conductive high-surface nanostructures as catalyst supports in conjunction with thin-film catalyst deposition. The presented study discusses unconventional technique of membrane electron assembly (MEA) preparation. Noble metal catalysts (Pt and Ir) were magnetron sputtered in very low loadings onto the surface of porous sublayers (located on gas diffusion layer or directly on membrane), forming so to say localized three-phase boundary. Ultrasonically sprayed corrosion resistant TiC-based sublayer was used as a support material on anode, whereas magnetron sputtered nanostructured etched nitrogenated carbon (CNx) served the same role on cathode. By using this configuration, we were able to significantly decrease the amount of noble metals (to thickness of just tens of nanometers), while keeping the performance comparable to that of average state-of-the-art catalysts. Complex characterization of prepared supported catalysts includes in-cell performance and durability tests, electrochemical impedance spectroscopy (EIS) as well as scanning electron microscopy (SEM) imaging and X-ray photoelectron spectroscopy (XPS) analysis. Our research proves that magnetron sputtering is a suitable method for thin-film deposition of electrocatalysts. Tested set-up of thin-film supported anode and cathode catalysts with combined loading of just 120 ug.cm⁻² yields remarkable values of specific current. Described approach of thin-film low-loading catalyst deposition might be relevant when noble metal reduction is the topmost priority.

Keywords: hydrogen economy, low-loading catalyst, magnetron sputtering, proton exchange membrane water electrolyzer

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Authors: J. J. Rickard, A. Belli, P. Goldberg Oppenheimer

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Medical diagnostics, environmental monitoring, homeland security and forensics increasingly demand specific and field-deployable analytical technologies for quick point-of-care diagnostics. Although technological advancements have made optical methods well-suited for miniaturization, a highly-sensitive detection technique for minute sample volumes is required. Raman spectroscopy is a well-known analytical tool, but has very weak signals and hence is unsuitable for trace level analysis. Enhancement via localized optical fields (surface plasmons resonances) on nanoscale metallic materials generates huge signals in surface-enhanced Raman scattering (SERS), enabling single molecule detection. This enhancement can be tuned by manipulation of the surface roughness and architecture at the sub-micron level. Nevertheless, the development and application of SERS has been inhibited by the irreproducibility and complexity of fabrication routes. The ability to generate straightforward, cost-effective, multiplex-able and addressable SERS substrates with high enhancements is of profound interest for SERS-based sensing devices. While most SERS substrates are manufactured by conventional lithographic methods, the development of a cost-effective approach to create nanostructured surfaces is a much sought-after goal in the SERS community. Here, a method is established to create controlled, self-organized, hierarchical nanostructures using electrohydrodynamic (HEHD) instabilities. The created structures are readily fine-tuned, which is an important requirement for optimizing SERS to obtain the highest enhancements. HEHD pattern formation enables the fabrication of multiscale 3D structured arrays as SERS-active platforms. Importantly, each of the HEHD-patterned individual structural units yield a considerable SERS enhancement. This enables each single unit to function as an isolated sensor. Each of the formed structures can be effectively tuned and tailored to provide high SERS enhancement, while arising from different HEHD morphologies. The HEHD fabrication of sub-micrometer architectures is straightforward and robust, providing an elegant route for high-throughput biological and chemical sensing. The superior detection properties and the ability to fabricate SERS substrates on the miniaturized scale, will facilitate the development of advanced and novel opto-fluidic devices, such as portable detection systems, and will offer numerous applications in biomedical diagnostics, forensics, ecological warfare and homeland security.

Keywords: hierarchical electrohydrodynamic patterning, medical diagnostics, point-of care devices, SERS

Procedia PDF Downloads 317