Search results for: crystalline

Authors: Babatunde Oluwole Ogunsile, Omosola Monisola Fasoranti

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High costs and toxicological hazards associated with the physicochemical methods of producing nanoparticles have limited their widespread use in clinical and biomedical applications. An ethically sound alternative is the utilization of plant bioresources as a low cost and eco–friendly biological approach. Silver nanoparticles (AgNPs) were synthesized from aqueous leaf extract of Tithonia diversifolia plant. The UV-Vis Spectrophotometer was used to monitor the formation of the AgNPs at different time intervals and different ratios of plant extract to the AgNO₃ solution. The biosynthesized AgNPs were characterized by FTIR, X-ray Diffraction (XRD) and Scanning Electron Microscope (SEM). Antimicrobial activities of the AgNPs were investigated against ten human pathogens using agar well diffusion method. The AgNPs yields were modeled using a second-order factorial design. The result showed that the rate of formation of the AgNPs increased with respect to time while the optimum ratio of plant extract to the AgNO₃ solution was 1:1. The hydroxyl group was strongly involved in the bioreduction of the silver salt as indicated by the FTIR spectra. The synthesized AgNPs were crystalline in nature, with a uniformly distributed network of the web-like structure. The factorial model predicted the nanoparticles yields with minimal errors. The nanoparticles were active against all the tested pathogens and thus have great potentials as antimicrobial agents.

Keywords: antimicrobial activities, green synthesis, silver nanoparticles, Tithonia diversifolia

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Authors: Rawan Aljabbari, Thamer Alomayri, Faisal G. Al-Maqate, Abeer Al Suwat

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For environmentally friendly innovative technologies and a sustainable future, fly ash/TiO₂ thin film nanocomposites are essential. Fly ash will be doped with titanium dioxide in this work in order to better understand its optical characteristics and employ it in semiconductor electrical devices. This study focused on the structure, morphology, and optical properties of fly ash/TiO₂ thin films. The spin-coating technique was used to create thin coatings of fly ash/TiO₂. For the first time, the doping of TiO₂ in the fly ash host at ratios of 1, 2, and 3 wt% was investigated with the thickness of all samples fixed. When compared to undoped thin films, the surface morphology of the doped thin films was improved. The weakly crystalline structure of the doped fly ash films was verified by XRD. The optical bandgap energy of these films was successfully reduced by the TiO₂ doping, going from 3.9 to 3.5 eV. With increasing dopant concentration, the value of Urbach energy is increasing. The optical band gap is clearly in opposition to the disorder. While it considerably improved the optical conductivity to a value of 4.1 x 10^9 s^(-1), it also raised the refractive index and extinction coefficient. Depending on the TiO₂ doping ratio, the transmittance decreased, and the reflection increased. As the TiO₂ concentration rises, the absorption of photon energy rises, and the absorption coefficient of photon energy is reduced. results in their possible use as solar energy and semiconductor materials.

Keywords: fly ash, structural analysis, optical properties, morphology

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Authors: Veronique Jubera, Guillaume Salek, Manuel Gaudon, Alain Garcia, Alain Demourgues

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Luminescence of transition metal and rare earth elements cover ultraviolet to far infrared wavelengths. Applications of phosphors are numerous. One can cite lighting, sensing, laser, energy, medical or military applications. But regarding each domain, specific criteria are required and they can be achieved with a strong control of the chemical composition. Emission of doped materials can be tailored with modifications of the local environment of the cations. For instance, the increase of the crystal field effect shifts the divalent manganese radiative transitions from the green to the red color. External factor as heat-treatment can induce changes of the doping element location or modify the unit cell crystalline symmetry. By controlling carefully the synthesis route, it is possible to initiate emission shift and to establish the thermal history of a compound. We propose to demonstrate through the luminescence of divalent manganese and trivalent rare earth doped oxide, that it is possible to follow the thermal history of a material. After optimization of the synthesis route, structural and optical properties are discussed. Finally, thermal calibration graphs are successfully established on these doped compounds. This makes these materials promising probe for thermal sensing.

Keywords: emission, thermal sensing, transition metal, rare eath element

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Authors: Khamael M. Abualnaja, Lidija Šiller, Ben R. Horrocks

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Metal enhanced luminescence of alkyl-capped silicon quantum dots (C11-SiQDs) was obtained by mixing C11-SiQDs with silver nanoparticles (AgNPs). C11-SiQDs have been synthesized by galvanostatic method of p-Si (100) wafers followed by a thermal hydrosilation reaction of 1-undecene in refluxing toluene in order to extract alkyl-capped silicon quantum dots from porous Si. The chemical characterization of C11-SiQDs was carried out using X-ray photoemission spectroscopy (XPS). C11-SiQDs have a crystalline structure with a diameter of 5 nm. Silver nanoparticles (AgNPs) of two different sizes were synthesized also using photochemical reduction of silver nitrate with sodium dodecyl sulphate. The synthesized Ag nanoparticles have a polycrystalline structure with an average particle diameter of 100 nm and 30 nm, respectively. A significant enhancement up to 10 and 4 times in the luminescence intensities was observed for AgNPs100/C11-SiQDs and AgNPs30/C11-SiQDs mixtures, respectively using 488 nm as an excitation source. The enhancement in luminescence intensities occurs as a result of the coupling between the excitation laser light and the plasmon bands of Ag nanoparticles; thus this intense field at Ag nanoparticles surface couples strongly to C11-SiQDs. The results suggest that the larger Ag nanoparticles i.e.100 nm caused an optimum enhancement in the luminescence intensity of C11-SiQDs which reflect the strong interaction between the localized surface plasmon resonance of AgNPs and the electric field forming a strong polarization near C11-SiQDs.

Keywords: silicon quantum dots, silver nanoparticles (AgNPs), luminescence, plasmon

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Authors: Waranya Pongpaiboon, Warangkana Srichamnong, Supat Chaiyakul

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Enzymatic modification of rice flour can produce highly functional derivatives use in food industries. This study aimed to evaluate the physical properties and resistant starch content of rice flour residues hydrolyzed by α-amylase. Rice flour hydrolyzed by α-amylase (60 and 300 u/g) for 1, 24 and 48 hours were investigated. Increasing enzyme concentration and hydrolysis time resulted in decreased rice flour residue’s lightness (L*) but increased redness (a*) and yellowness (b*) of rice flour residues. The resistant starch content and peak viscosity increased when hydrolysis time increased. Pasting temperature, trough viscosity, breakdown, final viscosity, setback and peak time of the hydrolyzed flours were not significantly different (p>0.05). The morphology of native flour was smooth without observable pores and polygonal with sharp angles and edges. However, after hydrolysis, granules with a slightly rough and porous surface were observed and a rough and porous surface was increased with increasing hydrolyzed time. The X-ray diffraction patterns of native flour showed A-type configuration, which hydrolyzed flour showed almost 0% crystallinity indicated that both amorphous and crystalline structures of starch were simultaneously hydrolyzed by α-amylase.

Keywords: α-Amylase, enzymatic hydrolysis, pasting properties, resistant starch

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Authors: Mladen Jankovic, Biljana Djuric, Djurdja Oljaca, Vladimir Damjanovic, Radislav Filipovic, Zoran Obrenovic

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One of the key characteristics of zeolites with ZSM-5 crystalline form is the possibility of synthesis in a wide range of molar ratios, from the relatively low ratio of about 20 to highly silicate forms with a Si/Al ratio over 1000. For industrial production and commercial use of this type of zeolite, it is very important to know the influence of the molar Si/Al ratio on the characteristics of zeolite powders. In this paper, the influence of the Si/Al ratio on the characteristics of H-ZSM-5 zeolites synthesized in the presence of tetrapropylammonium bromide is questioned, including the possibility of conversion to the H-form using different acids. The quality of the samples is characterized in terms of crystallinity, chemical composition, morphology, granulometry, specific surface area (BET), pore size and acidity. XRD, FT-IR, EDX, ICP, SEM and TPD instrumental techniques were used to characterize the samples. In most of the performed syntheses, zeolite has been obtained with very good properties. It was shown that the examined conditions have a significant influence on the characteristics of the synthesized powders. The different chemical composition of the starting mixture, ie. the Si/Al ratio, has a very significant influence on the crystal structure of the synthesized powders, and thus on the other tested characteristics. It has been observed that optimal ion exchange results for powders of different Si/Al ratios are achieved by using different acids. Also, the dependence of the specific surface on the concentration of H+ or Na+ ions was confirmed.

Keywords: Characterisation, H-ZSM-5, molar ratio, synthesis, tetrapropylammonium bromide

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Authors: Ibrahim Abdelfattah, Adel Ismail, Ahmed Helal, Mohamed Faisal

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Advanced oxidation technologies are an environment friendly approach for the remediation of industrial wastewaters. Here, one pot synthesis of mesoporous In₂O₃-TiO₂ nanocomposites at different In₂O₃ contents (0-3 wt%) have been synthesized through a facile sol-gel method to evaluate their photocatalytic performance for the degradation of the imazapyr herbicide and phenol under visible light and UV illumination compared with commercially available either Degussa P-25 or UV-100 Hombikat. The prepared mesoporous In₂O₃-TiO₂ nanocomposites were characterized by TEM, STEM, XRD, Raman FT-IR, Raman spectra and diffuse reflectance UV-visible. The bandgap energy of the prepared photocatalysts was derived from the diffuse reflectance spectra. XRD Raman's spectra confirmed that highly crystalline anatase TiO₂ phase was formed. TEM images show TiO₂ particles are quite uniform with 10±2 nm sizes with mesoporous structure. The mesoporous TiO₂ exhibits large pore volumes of 0.267 cm³g⁻¹ and high surface areas of 178 m²g⁻¹, but they become reduced to 0.211 cm³g⁻¹ and 112 m²g⁻¹, respectively upon In₂O₃ incorporation, with tunable mesopore diameter in the range of 5 - 7 nm. The 0.5% In₂O₃-TiO₂ nanocomposite is considered to be the optimum photocatalyst which is able to degrade 90% of imazapyr herbicide and phenol along 180 min and 60 min respectively. The proposed mechanism of this system and the role of In₂O₃ are explained by details.

Keywords: In₂O₃-TiO₂ nanocomposites, sol-gel method, visible light illumination, UV illumination, herbicide and phenol wastewater, removal

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Authors: Abigail Parra Parra, Jorge L. Morelos Hernandez, Pedro A. Marquez Agilar, Marina Vlasova, Jesus Colin De La Cruz

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Carbothermal reduction of metal oxides is widely used both in metallurgical processes and in the production of oxygen-free refractory ceramics. As a rule, crushed coke and graphite are used as a reducing agent. The products of carbonization of organic compounds are among the innovative reducing agents. The aim of this work was to study the process of reduction of iron oxide (hematite) down to iron by waste active sludge (WAS) carbonization products. WAS was chosen due to the accumulation of a large amount of this type of waste, soil pollution, and the relevance of the development of technologies for its disposal. The studies have shown that the temperature treatment of mixtures WAS-Fe₂O₃ in the temperature range 900-1000 ºC for 1-5 hours under oxygen deficiency is described by the following scheme: WAS + Fe₂O₃→ C,CO + Fe₂O₃→ C + FexO → Fe (amorphous and crystalline). During the heat treatment of the mixtures, strong samples are formed. The study of the electrical conductive properties of such samples showed that, depending on the ratio of the components in the initial mixtures, it is possible to change the values of electrical resistivity from 5.6 Ω‧m to 151.6 Ω‧m When a current is passed through the samples, they are heated from 240 to 378ºC. Thus, based on WAS-Fe₂O₃ mixtures, heating elements can be created that can be used to heat ceramics and concrete.

Keywords: Fe₂O₃, reduction, waste activate sludge, electroconductivity

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Authors: Lucas Viani, Benedetta Mennucci, Soo Young Park, Johannes Gierschner

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Organic semiconductors have attracted the attention of the scientific community in the past decades due to their unique physicochemical properties, allowing new designs and alternative device fabrication methods. Until today, organic electronic devices are largely based on conjugated polymers mainly due to their easy processability. In the recent years, due to moderate ET and CT efficiencies and the ill-defined nature of polymeric systems the focus has been shifting to small conjugated molecules with well-defined chemical structure, easier control of intermolecular packing, and enhanced CT and ET properties. It has led to the synthesis of new small molecules, followed by the growth of their crystalline structure and ultimately by the device preparation. This workflow is commonly followed without a clear knowledge of the ET and CT properties related mainly to the macroscopic systems, which may lead to financial and time losses, since not all materials will deliver the properties and efficiencies demanded by the current standards. In this work, we present a theoretical workflow designed to predict the key properties of ET of these new materials prior synthesis, thus speeding up the discovery of new promising materials. It is based on quantum mechanical, hybrid, and classical methodologies, starting from a single molecule structure, finishing with the prediction of its packing structure, and prediction of properties of interest such as static and averaged excitonic couplings, and exciton diffusion length.

Keywords: organic semiconductor, organic crystals, energy transport, excitonic couplings

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Authors: J. K. Adedeji, S. T. Ijatuyi

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The application of neural network using pattern recognition to study the fluid dynamics and predict the groundwater reservoirs properties has been used in this research. The essential of geophysical survey using the manual methods has failed in basement environment, hence the need for an intelligent computing such as predicted from neural network is inevitable. A non-linear neural network with an XOR (exclusive OR) output of 8-bits configuration has been used in this research to predict the nature of groundwater reservoirs and fluid dynamics of a typical basement crystalline rock. The control variables are the apparent resistivity of weathered layer (p₁), fractured layer (p₂), and the depth (h), while the dependent variable is the flow parameter (F=λ). The algorithm that was used in training the neural network is the back-propagation coded in C++ language with 300 epoch runs. The neural network was very intelligent to map out the flow channels and detect how they behave to form viable storage within the strata. The neural network model showed that an important variable g_r (gravitational resistance) can be deduced from the elevation and apparent resistivity p_a. The model results from SPSS showed that the coefficients, a, b and c are statistically significant with reduced standard error at 5%.

Keywords: gravitational resistance, neural network, non-linear, pattern recognition

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Authors: Rym Sassi, Franck Fayon, Mohend Chaouche, Emmanuel Veron, Valerie Montouillout

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The chemical phenomena occurring during cement hydration are complex and interdependent, and even after almost two centuries of studies, they are still difficult to solve for complex mixtures combining different hydraulic binders. Powder-XRD has been widely used for characterizing the crystalline phases in both anhydrous and hydrated cement, but only limited information is obtained in the case of strongly disordered and amorphous phases. In contrast, local spectroscopies like solid-state NMR can provide a quantitative description of noncrystalline phases. In this work, the structural modifications occurring during hydration of a fast-setting ternary binder based on white Portland cement, white calcium aluminate cement, and calcium sulfate were investigated using advanced solid-state NMR methods. We particularly focused on the early stage of the hydration up to 28 days, working with samples whose hydration was controlled and stopped. ²⁷Al MQ-MAS as well as {¹H}-²⁷Al and {¹H}-²⁹Si Cross- Polarization MAS NMR techniques were combined to distinguish all of the aluminum and silicon species formed during the hydration. The NMR quantification of the different phases was conducted in parallel with the XRD analyses. The consumption of initial products, as well as the precipitation of hydraulic phases (ettringite, monosulfate, strätlingite, CSH, and CASH), were unambiguously quantified. Finally, the drawing of the consumption and formation of phases was correlated with mechanical strength measurements.

Keywords: cement, hydration, hydrates structure, mechanical strength, NMR

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Authors: S. Palaniyappan, P. K. Chennam, M. Trautmann, H. Ahmad, T. Mehner, T. Lampke, G. Wagner

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In structural-health monitoring of fiber reinforced plastics (FRPs), every single inorganic fiber sensor that are integrated into the bulk material requires an electrical insulation around itself, when the surrounding reinforcing fibers are electrically conductive. This results in a more accurate data acquisition only from the sensor fiber without any electrical interventions. For this purpose, thin nano-films of aluminium oxide (Al₂O₃)-based electrical-insulation coatings have been fabricated around the Silicon Carbide (SiC) single fiber sensors through reactive DC magnetron sputtering technique. The sputtered coatings were amorphous in nature and the thickness of the coatings increased with an increase in the sputter time. Microstructural characterization of the coated fibers performed using scanning electron microscopy (SEM) confirmed a homogeneous circumferential coating with no detectable defects or cracks on the surface. X-ray diffraction (XRD) analyses of the as-sputtered and 2 hours annealed coatings (825 & 1125 ˚C) revealed the amorphous and crystalline phases of Al₂O₃ respectively. Raman spectroscopic analyses produced no characteristic bands of Al₂O₃, as the thickness of the films was in the nanometer (nm) range, which is too small to overcome the actual penetration depth of the laser used. In addition, the influence of the insulation coatings on the mechanical properties of the SiC sensor fibers has been analyzed.

Keywords: Al₂O₃ thin film, electrical insulation coating, PVD process, SiC fibre, single fibre tensile test

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Authors: Meltem Bolluk, Ismail Duman

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Boron exhibits the properties of high melting temperature (2273K to 2573 K), high hardness (Mohs: 9,5), low density (2,340 g/cm3), high chemical resistance, high strength, and semiconductivity (band gap:1,6-2,1 eV). These superior properties enable to use it in several high-tech areas from electronics to nuclear industry and especially in high temperature metallurgy. Amorphous boron and crystalline boron have different application areas. Amorphous boron powder (directly amorphous and/or α-rhombohedral) is preferred in rocket firing, airbag inflating and in fabrication of superconducting MgB2 wires. The conventional ways to produce elemental boron with a purity of 85 pct to 95 prc are metallothermic reduction, fused salt electrolysis and mechanochemical synthesis; but the only way to produce high-purity boron powders is Chemical Vapour Deposition (Hot Surface CVD). In this study; amorphous boron powders with a minimum purity of 99,9 prc were synthesized in quartz tubes using BCl3-H2 gas mixture by CVD. Process conditions based on temperature and gas flow rate were determined. Thermodynamical interpretation of BCl3-H2 system for different temperatures and molar rates were performed using Fact Sage software. The characterization of powders was examined by using Xray diffraction (XRD), Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM), Stereo Microscope (SM), Helium gas pycnometer analysis. The purities of final products were determined by titration after lime fusion.

Keywords: amorphous boron, CVD, powder production, powder characterization

Procedia PDF Downloads 189

Authors: Maha Al-Ali, Selvakannan Periasamy, Rajarathinam Parthasarathy

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Drying temperature is an important factor impacting the physicochemical properties of the dried materials, particularly the pharmaceutical powders. Drying of pharmaceuticals by using microwave radiation is very limited, and the available information about the interaction between the electromagnetic radiations and the pharmaceutical material is still scarce. Therefore, microwave drying process is employed in this work to dry the wet (moisturised) granules of the formulated naproxen-sodium drug. This study aims to investigate the influences of the microwave radiation temperatures on the moisture removal, the crystalline structure, the size and morphology of the dried naproxen-sodium particles, and identify any potential changes in the chemical groups of the drug. In this work, newly formulated naproxen-sodium is prepared and moisturized by wet granulation process and hence dried by using microwave radiation at different temperatures. Moisture analyzer, Fourier-transform infrared spectroscopy, powder X-ray diffraction, and scanning electron microscope are used to characterise the non-moisturised powder (reference powder), the moisturised granules, and the dried particles. The results show that microwave drying of naproxen-sodium at high drying temperature is more efficient than that at low temperatures in terms of the moisture removal. Although there is no significant change in the chemical structure of the dried particles, the particle size, crystallinity and morphology are relatively changed with changing of heating temperature.

Keywords: heating temperature, microwave drying, naproxen-sodium, particle size

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Authors: Srutirekha Giri, Manoranjan Sahoo, Anuradha Das, Pravanjan Mallick, Biswajit Mallick

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Ion Beam (IB) technique is a very powerful experimental technique for both material synthesis and material modifications. In this work, 3MeV proton beam was generated using the 3MV Tandem machine of the Institute of Physics, Bhubaneswar and extracted into air for the irradiation-induced modification purpose[1]. The polymeric material can be modeled for a three-phase system viz. crystalline(I), amorphous(II) and mesomorphic(III). So far, our knowledge is concerned. There are only few techniques reported for the synthesis of this third-phase(III) of polymer. The IB induced technique is one of them and has been reported very recently [2-4]. It was observed that by irradiating polyethylene terephthalate (PET) fiber at very low proton fluence, 10¹⁰ - 10¹² p/s, possess 2D mesophase structure. This was confirmed using X-ray diffraction technique. A low-intensity broad peak was observed at small angle of about 2θ =6º, when the fiber axis was mounted parallel to the X-ray direction. Such peak vanished in the diffraction spectrum when the fiber axis was mounted perpendicular to the beam direction. The appearance of this extra peak in a particular orientation confirms that the phase is 2-dimensionally oriented (mesophase). It is well known that the mesophase is a 2-dimensionally ordered structure but 3-dimensionally disordered. Again, the crystallite of the mesophase peak particle was measured about 3nm. The MeV proton-induced 2D mesophase patterning of nanocrystallites (3nm) of PET due to irradiation was observed within the above low fluence range and failed in high proton fluence. This is mainly due to the breaking of crystallites, radiation-induced thermal degradation, etc.

Keywords: Ion irradiation, mesophase, nanocrystallites, polymer

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Authors: Uchechukwu Vincent Okpala

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Under the Sun, energy is a key factor for the sustenance of life and its environment. The need to protect the environment as energy is generated and consumed has called for renewable and green energy sources. To be part of this green revolution, we synthesized and characterized undoped and velvet tamarind doped zinc sulfide (ZnS) crystals using sol-gel methods. Velvet tamarind was whittled down using the top-down approach of nanotechnology. Sodium silicate, tartaric acid, zinc nitrate, and thiourea were used as precursors. The grown samples were annealed at 105°C. Structural, optical, and compositional analyses of the grown samples revealed crystalline structures with varied crystallite sizes influenced by doping. Energy-dispersive X-ray spectroscopy confirmed elemental compositions of Zn, S, C and O in the films. Atomic percentages of the elements varied with VT doping. FT-IR analysis indicated the presence of functional groups like O-H stretching (alcohol), C=C=C stretching (alkene group), C=C bending, C-H stretching (alkane), N-H stretching (aliphatic primary amine) and N=C=S stretching (isothiocyanate) constituent in the film. The transmittance of the samples increased from the visible region to the infrared region making the samples good for poultry and solar energy applications. The bandgap energy of the films decreased as the number of VT drops increased, from 2.4 to 2.2. They were wide band gap materials and were good for optoelectronic, photo-thermal, high temperature, high power and solar cell applications.

Keywords: doping, sol-gel, velvet tamarind, ZnS.

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Authors: Muhammad Jawad Saleem, Faisal Hafeez, Muhammad Arshad, Afifa Naeem, Ayesha Iftekhar

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Bacillus thuringiensis is a gram-positive spore-forming bacterium that belongs to the Bacillus cereus group of Bacilli and it produces ICP (insecticidal crystal protein) Cry toxins or Cysts toxins. Spores are produced as parasporal crystalline inclusions bodies (also known as endotoxins) at the onset of sporulation during the stationary growth phase. During vegetative growth that does not form crystals and is called vegetative insecticidal proteins (VIP) and secreted an insecticidal protein (SIP). Bacillus thuringiensis (Bt) is important for pest management either in the form of insecticides or through incorporated in the gene of the crop. Bioassays were conducted on the F2 generation of 1st instar larvae of H. armigera by the diet incorporation method to determine the susceptibility to Bt Cry toxins (Cry1Ac, Cry2Ab, Cry2A). The median lethal concentration (LC₅₀) of Cry1Ac, Cry2Ab, Cry2A ranged from 0.11 to 1.06 µg/ml and moult inhibitory concentration (MIC₅₀) of Cry1Ac, Cry2Ab, Cry2A ranged from 0.05 to 0.25 µg/ml. Cry1Ac was found most toxic to 1st instar larvae of H. armigera as compared to other Bt Cry toxins (Cry1Ac, Cry2Ab, Cry2A). The experimental results are important to policy-makers and technology providers to develop strategies for the exploitation of transgenic Bt cotton varieties as a component of integrated pest management.

Keywords: Bt toxin, Cry1Ac, Cry2Ab, Cry2A, susceptibility, Helicoverpa armigera

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Authors: Débora N. Zambrano, Marina O. Gosatti, Leandro M. Dufou, Daniel A. Serrano, M. Mónica Guraya, Soledad Perez-Catán

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Nanoporous g-Al₂O₃ samples were synthesized via a sol-gel technique, introducing changes in the Yoldas´ method. The aim of the work was to achieve an effective control of the nanostructure properties and morphology of the final g-Al₂O₃. The influence of the reagent temperature during the hydrolysis was evaluated in case of water at 5 ºC and 98 ºC, and alkoxide at -18 ºC and room temperature. Sol-gel transitions were performed at 120 ºC and room temperature. All g-Al₂O₃ samples were characterized by X-ray diffraction, nitrogen adsorption and thermal analysis. Our results showed that temperature of both water and alkoxide has not much influence on the nanostructure of the final g-Al₂O₃, thus giving a structure very similar to that of samples obtained by the reference method as long as the reaction temperature above 75 ºC is reached soon enough. XRD characterization showed diffraction patterns corresponding to g-Al₂O₃ for all samples. Also BET specific area values (253-280 m²/g) were similar to those obtained by Yoldas’s original method. The temperature of the sol-gel transition does not affect the resulting sample structure, and crystalline boehmite particles were identified in all dried gels. We analyzed the reproducibility of the samples’ structure by preparing different samples under identical conditions; we found that performing the sol-gel transition at 120 ºC favors the production of more reproducible samples and also reduces significantly the time of the sol-gel reaction.

Keywords: nanostructure alumina, boehmite, sol-gel technique, N2 adsorption/desorption isotherm, pore size distribution, BET area.

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Authors: Erdem Elibol, Musa Cadırcı, Nedim Tutkun

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Recently, colloidal quantum dots (CQDs) have drawn increasing attention due to their unique size tunability, which makes them potential candidates for numerous applications including photovoltaic, LEDs, and imaging. However, the main challenge to exploit CQDs properly is that there has not been an effective method to produce them with highly crystalline form and narrow size dispersion. Hot injection method is one of the widely used techniques to produce high-quality nanoparticles. In this method, the key parameter is to reduce the time for injection of the precursors into each other, which yields fast and constant nucleation rate and hence to highly monodisperse QDs. In conventional hot injection method, the injection of precursors is carried out using standard lab syringes with long needles. However, this technique is relatively slow and thus will result in poor optical properties in QDs. In this work, highly luminescent CdTe QDs were synthesised by transferring hot precursors into each other using cannula method. Unlike regular syringe technique, with the help of high pressure difference between two precursors’ flasks and wide cross-section of cannula, the hot cannulation process is too short which yields narrow size distribution and high quantum yield of CdTe QDs. Here QDs with full width half maximum (FWHM) of 28 nm was achieved. In addition, the photoluminescence quantum yield of our samples was measured to be about 21 ± 0.9 which is at least twice the previous record values for CdTe QDs wherein syringe was used to transfer precursors.

Keywords: CdTe, hot injection method, luminescent, quantum dots

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Authors: Peter K. Galenko, Stefanie Koch, Markus Rettenmayr, Robert Wonneberger, Evgeny V. Kharanzhevskiy, Maria Zamoryanskaya, Vladimir Ankudinov

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We analyze the structure of undercooled melts, crystal growth kinetics and amorphous/crystalline microstructure of rapidly solidifying glass-forming Pd-based and CuZr-based alloys. A dendrite growth model is developed using a combination of the kinetic phase-field model and mesoscopic sharp interface model. The model predicts features of crystallization kinetics in alloys from thermodynamically controlled growth (governed by the Gibbs free energy change on solidification) to the kinetically limited regime (governed by atomic attachment-detachment processes at the solid/liquid interface). Comparing critical undercoolings observed in the crystallization kinetics with experimental data on melt viscosity, atomistic simulation's data on liquid microstructure and theoretically predicted dendrite growth velocity allows us to conclude that the dendrite growth kinetics strongly depends on the cluster structure changes of the melt. The obtained data of theoretical and experimental investigations are used for interpretation of microstructure of samples processed in electro-magnetic levitator on board International Space Station in the frame of the project "MULTIPHAS" (European Space Agency and German Aerospace Center, 50WM1941) and "KINETIKA" (ROSKOSMOS).

Keywords: dendrite, kinetics, model, solidification

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Authors: Dilip Depan, Austin Simoneaux, William Chirdon, Ahmed Khattab

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In this study, we present a novel approach to synthesize polymer nanocomposites with nanohybrid shish-kebab architecture (NHSK). For this low-density and high density polyethylene (PE) was crystallized on various carbon nano-fillers using a novel and convenient method to prepare high-yield NHSK. Polymer crystals grew epitaxially on carbon nano-fillers using a solution crystallization method. The mixture of polymer and carbon fillers in xylene was flocculated and precipitated in ethanol to improve the product yield. Carbon nanofillers of varying diameter were also used as a nucleating template for polymer crystallization. The morphology of the prepared nanocomposites was characterized scanning electron microscopy (SEM), while differential scanning calorimetry (DSC) was used to quantify the amount of crystalline polymer. Interestingly, whatever the diameter of the carbon nanofiller is, the lamellae of PE is always perpendicular to the long axis of nanofiller. Surface area analysis was performed using BET. Our results indicated that carbon nanofillers of varying diameter can be used to effectively nucleate the crystallization of polymer. The effect of molecular weight and concentration of the polymer was discussed on the basis of chain mobility and crystallization capability of the polymer matrix. Our work shows a facile, rapid, yet high-yield production method to form polymer nanocomposites to reveal application potential of NHSK architecture.

Keywords: carbon nanotubes, polyethylene, nanohybrid shish-kebab, crystallization, morphology

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Authors: S. Patel, T. Mitra, R. Dubey, J. Keller

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In the present investigations, an attempt has been made to study the charge storage mechanism and mechanism for the flow of transient charging and discharging current in an amorphous polymer (Polysulfone) (PSF) and a semi-crystalline polar Polyvinylidene fluoride (PVDF) blends in ratio PSF: PVDF: 80:20;85:15;90:10 and 95:05 at various poling temperatures (i.e. 60, 75, 90 and 1150C) and with field strength (100, 150, 200 and 250kVcm⁻¹). Thermally stimulated depolarizing current TSDC thermograms for (Polysulfone (PSF) and Polyvinylidene fluoride (PVDF) Blends sample have been obtained under different polarizing conditions. Peaks are found at high-temperature side. The variation of structure on blending and poling condition affects the magnitude of TSDC. The activation energy values have been calculated using the initial rise method of Garlick and Gibson. The transient current with the similar polarizing condition has been investigated over a period of 3X10³ sec. The observed characteristics obey Curie-Von Schweidler law in the studied temperature range. The charging current versus polarizing temperature curves at a constant time, i.e., isochronal current characteristics were studied and the activation energies were calculated. The activation energy in transient thermograms calculated by different methods is in good agreement with the values obtained from TSDC studies.

Keywords: activation energy, polysulfone (PSF), polyvinylidenefluoride (PVDF), thermally stimulated depolarizing current (TSDC)

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Authors: Collins C. Chiemeke, A. Onugba, P. Sule

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High resolution seismic reflection has recently been carried out on Zaria batholith, with the aim of characterizing the granitic Zaria batholiths in terms of its lithology. The geology of the area has revealed that the older granite outcrops in the vicinity of Zaria are exposures of a syntectonics to late-tectonic granite batholiths which intruded a crystalline gneissic basement during the Pan-African Orogeny. During the data acquisition the geophone were placed at interval of 1 m, variable offset of 1 and 10 m was used. The common midpoint (CMP) method with 12 fold coverage was employed for the survey. Analysis of the generated 3D surface of the p wave velocities from different profiles for densities and bulk modulus revealed that the rock material is more consolidated in South East part of the batholith and less consolidated in the North Western part. This was in conformity with earlier identified geology of the area, with the South Eastern part majorly of granitic outcrop, while the North Western part is characterized with the exposure of gneisses and thick overburden cover. The difference in lithology was also confirmed by the difference in seismic sections and Arial satellite photograph. Hence two major lithologies were identified, the granitic and gneisses complex which are characterized by gradational boundaries.

Keywords: basement complex, batholith, high resolution, lithologies, seismic reflection

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Authors: Jonathan Galvan-Colin, Ariel Valladares, Renela Valladares, Alexander Valladares

Abstract:

Both porous materials and bulk metallic glasses have been studied due to their potential applications and their exceptional physical and chemical properties. However, each material presents certain drawbacks which have been thought to be overcome by generating bulk metallic glass foams (BMGF). Although some experimental reports have been performed on multicomponent BMGF, still no ab initio works have been published, as far as we know. We present an approach based on the expanding lattice (EL) method to generate binary amorphous nanoporous Cu64Zr36. Starting from two different configurations: a 108-atom crystalline cubic supercell (cCu64Zr36) and a 108-atom amorphous supercell (aCu64Zr36), both with an initial density of 8.06 g/cm3, we applied EL method to halve the density and to get 50% of porosity. After the lattice expansion the supercells were subject to ab initio molecular dynamics for 500 steps at constant room temperature. Then, the samples were geometry-optimized and characterized with the pair and radial distribution functions, bond-angle distributions and a coordination number analysis. We found that pores appeared along specific spatial directions different from one to another and that they differed in size and form as well, which we think is related to the initial structure. Due to the lack of experimental counterparts our results should be considered predictive and further studies are needed in order to handle a larger number of atoms and its implication on pore topology.

Keywords: ab initio molecular dynamics, bulk mettalic glass, porous alloy

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Authors: Rudra Vaghela, P. K. Kulkarni

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The aim of the present research was to develop oral Amphotericin B (AmB) nanocrystals (Nc) grafted with suitable ligand in order to enhance drug transport across the intestinal epithelial barrier and subsequently, active uptake by macrophages. AmB Nc were prepared by liquid anti-solvent precipitation technique (LAS). Poloxamer 188 was used to stabilize the prepared AmB Nc and grafted with mannose for actively targeting M cells in Peyer’s patches. To prevent shedding of the stabilizer and ligand, N,N’-Dicyclohexylcarbodiimide (DCC) was used as a cross-linker. The prepared AmB Nc were characterized for particle size, PDI, zeta potential, X-ray diffraction (XRD) and surface morphology using scanning electron microscope (SEM) and evaluated for drug content, in vitro drug release and cell uptake studies using caco-2 cells. The particle size of stabilized AmB Nc grafted with WGA was in the range of 287-417 nm with negative zeta potential between -18 to -25 mV. XRD studies revealed crystalline nature of AmB Nc. SEM studies revealed that ungrafted AmB Nc were irregular in shape with rough surface whereas, grafted AmB Nc were found to be rod-shaped with smooth surface. In vitro drug release of AmB Nc was found to be 86% at the end of one hour. Cellular studies revealed higher invasion and uptake of AmB Nc towards caco-2 cell membrane when compared to ungrafted AmB Nc. Our findings emphasize scope on developing oral delivery system for passively targeting M cells in Peyer’s patches.

Keywords: leishmaniasis, amphotericin b nanocrystals, macrophage targeting, LAS technique

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Authors: Sirwan Kamal, Hsein Kew, Hamid Jahromi

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This paper reports results of a study conducted to investigate strength, sorptivity, and permeability under pressure of concrete specimens, cured using a water-based curing compound. The specimens are treated with waterproofing admixtures or surface treatments to enhance performance while exposed to water. Four types of concrete specimens were prepared in the laboratory, Portland cement (CEM I), Portland-fly ash (CEM II/A-V), Blast-furnace cement (CEM III) and Portland-silica fume (CEM II/A-D). Concrete cubes were de-molded three hours after casting, and sprayed with a curing compound. Admixtures were added to the mix during batching, whereas surface treatments were applied on concrete after 28 days. Compressive strength test was carried out to assess the efficiency of curing compound to develop required strength. In addition, sorptivity and permeability tests were conducted to evaluate the performance of treated specimens with respect to water ingress. Results show that strength development in specimens cured with curing compound achieved up to 96% and 90% at 7 and 28 days respectively, compared to cubes cured in water. Moreover, specimens treated with waterproofing admixtures or surface treatments materials characterized by hydrophobic impregnation considerably reduced water penetration compared to untreated control cubes. On the other hand, cubes treated with admixtures or surface treatments materials characterized by crystalline effect were ineffective in reducing water penetration.

Keywords: admixtures, concrete, curing compound, surface treatments

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Authors: Schirin Hanf, Carlos Lizandara-Pueyo, Timmo P. Emmert, Ivana Jevtovikj, Roger Gläser, Stephan A. Schunk

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Metal alkoxides are very versatile precursors for a broad array of complex functional materials. However, metal alkoxides, especially transition metal alkoxides, tend to form oligomeric structures due to the very strong M–O–M binding motif. This fact hinders their facile application in sol-gel-processes and complicates access to complex carbonate or oxidic compounds after hydrolysis of the precursors. Therefore, the development of a synthetic alternative with the aim to grant access to carbonates and hydroxycarbonates from simple metal alkoxide precursors via hydrolysis is key to this project. Our approach involves the reaction of metal alkoxides with unsaturated isoelectronic molecules, such as carbon dioxide. Subsequently, a stoichiometric insertion of the CO₂ into the alkoxide M–O bond takes place and leads to the formation of soluble metal alkyl carbonates. This strategy is a very elegant approach to solubilize metal alkoxide precursors to make them accessible for sol-gel chemistry. After hydrolysis of the metal alkyl carbonates, crystalline metal carbonates, and hydroxycarbonates can be obtained, which were then utilized for the synthesis of Cu/Zn based bulk catalysts for methanol synthesis. Using these catalysts, a comparable catalytic activity to commercially available MeOH catalysts could be reached. Based on these results, a complement for traditional precipitation techniques, which are usually utilized for the synthesis of bulk methanol catalysts, have been found based on an alternative solubilization strategy.

Keywords: metal alkoxides, metal carbonates, metal hydroxycarbonates, CO₂ insertion, solubilization

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Authors: Bastola Narayan, Rajeev Ranjan

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The morphotropic phase boundary (MPB) in the magnetoelectric (1-x)BiFeO3-(x)PbTiO3 has remained a matter of controversy ever since its discovery in 1964. The nature of the phase stabilized (single phase tetragonal or coexistence of tetragonal and rhombohedral phases) is very sensitive to the slight changes in the synthesis conditions. It thus remained an enigma as to what is the essential physical factor which is controlled by the slight difference in the synthesis conditions that finally determines, whether the phase formed will be single phase or coexistence of phases. In this paper, we demonstrate that the nature of the phase stabilized in this system is uniquely dependent on the crystallite size. The system is shown to exhibit features of abnormal grain growth (AGG) during sintering with abrupt increase in the grain size from ~ 1 micron to ~ 10 microns. The 10 micron grains exhibit pure tetragonal phase while the 1 micron grains exhibit coexistence of rhombohedral and tetragonal ferroelectric phases. The Rietveld analysis of powder neutron diffraction shows a paramagnetic to antiferromagnetic order transition inducing with crystalline size reduction from 10 micron to 1 micron. Since tetragonal phase is known to have paramagnetic order and rhombohedral phase has antiferromagnetic order in room temperature, this further strengthens our argument of size induced structure transition.

Keywords: size driven MPB, size driven magnetic ordering, abnormal grain growth, phase formation in BF-PT system

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Authors: Darlington Ashiegbu, Herman Johannes Potgieter

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The increasing utilization of Zinc Oxide (ZnO) as a better alternative to TiO₂ has been attributed to its wide bandgap (3.37eV), lower production cost, ability to absorb over a larger range of the UV-spectrum and higher efficiency in some cases. ZnO nanoparticles were synthesized via sol-gel process and calcined at 400ᵒC, 500ᵒC, and 650ᵒC. The as-synthesized nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and Brunauer–Emmett–Teller (BET) surface area measurement. Scanning electron micrograph revealed pseudo-spherical and rod-like morphologies and a high rate of agglomeration for the sample calcined at 650ᵒC, Brunnauer Emmett Teller (BET) surface area measurement was highest in the sample calcined at 500ᵒC, energy dispersive X-ray spectroscopy (EDS) results confirmed the purity of the samples as only Zn and O₂ were detected and X-ray diffraction (XRD) results revealed crystalline hexagonal wurtzite structure of the ZnO nanoparticles. All three samples were utilized in the degradation of ethylbenzene, and a UV-Vis spectrophotometer was utilized in monitoring degradation of ethylbenzene. The sample calcined at 500ᵒC had the highest surface area for reaction, lowest agglomeration and the highest photocatalytic activity in the degradation of ethylbenzene. This revealed temperature as a very important factor in improved and higher photocatalytic activity.

Keywords: ethylbenzene, pseudo-spherical, sol-gel, zinc oxide

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Authors: Kkochorong Park, Keun Cheon Kim, Hyoban Lee, Eun Ju Lee, Bongsoo Kim

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Introduction of biomaterials such as DNA, RNA, proteins is important for many research areas. There are many methods to introduce biomaterials into living organisms like tissue and cells. To introduce biomaterials, several indirect methods including virus‐mediated delivery, chemical reagent (i.e., lipofectamine), electrophoresis have been used. Such methods are passive delivery using an endocytosis process of cell, reducing an efficiency of delivery. Unlike the indirect delivery method, it has been reported that a direct delivery of exogenous biomolecules into nucleus have been more efficient to expression or integration of biomolecules. Nano-sized material is beneficial for detect signal from cell or deliver stimuli/materials into the cell at cellular and molecular levels, due to its similar physical scale. Especially, because 1 dimensional (1D) nanomaterials such as nanotube, nanorod and nanowire with high‐aspect ratio have nanoscale geometry and excellent mechanical, electrical, and chemical properties, they could play an important role in molecular and cellular biology. In this study, by using single crystalline 1D noble metal nanowire, we fabricated nano-sized 1D injector which can successfully interface with living cells and directly deliver biomolecules into several types of cell line (i.e., stem cell, mammalian embryo) without inducing detrimental damages on living cell. This nano-bio technology could be a promising and robust tool for introducing exogenous biomaterials into living organism.

Keywords: DNA, gene delivery, nanoinjector, nanowire

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