Search results for: silver nanoparticles (AgNPs)

Authors: Aleksandra Boldyreva, Alexander Golubnichiy, Artem Abakumov

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Various perovskite materials have surprisingly high resistance towards high-energy electrons, protons, and hard ionization, such as X-rays and gamma-rays. Superior radiation hardness makes a family of perovskite semiconductors an attractive candidate for single- and multijunction solar cells for the space environment and as X-ray and gamma-ray detectors. One of the methods to study the radiation hardness of different materials is by exposing them to gamma photons with high energies (above 500 keV) Herein, we have explored the recombination dynamics and defect concentration of a mixed cation mixed halide perovskite Cs0.17FA0.83PbI1.8Br1.2 with 1.74 eV bandgap after exposure to a gamma-ray source (2.5 Gy/min). We performed an advanced STEM EDX analysis to reveal different types of defects formed during gamma exposure. It was found that 10 kGy dose results in significant improvement of perovskite crystallinity and homogeneous distribution of I ions. While the absorber layer withstood gamma exposure, the hole transport layer (PTAA) as well as indium tin oxide (ITO) were significantly damaged, which increased the interface recombination rate and reduction of fill factor in solar cells. Thus, STEM analysis is a powerful technique that can reveal defects formed by gamma exposure in perovskite solar cells. Methods: Data will be collected from perovskite solar cells (PSCs) and thin films exposed to gamma ionisator. For thin films 50 μL of the Cs0.17FA0.83PbI1.8Br1.2 solution in DMF was deposited (dynamically) at 3000 rpm followed by quenching with 100 μL of ethyl acetate (dropped 10 sec after perovskite precursor) applied at the same spin-coating frequency. The deposited Cs0.17FA0.83PbI1.8Br1.2 films were annealed for 10 min at 100 °C, which led to the development of a dark brown color. For the solar cells, 10% suspension of SnO2 nanoparticles (Alfa Aesar) was deposited at 4000 rpm, followed by annealing on air at 170 ˚C for 20 min. Next, samples were introduced into a nitrogen glovebox for the deposition of all remaining layers. Perovskite film was applied in the same way as in thin films described earlier. Solution of poly-triaryl amine PTAA (Sigma Aldrich) (4 mg in chlorobenzene) was applied at 1000 rpm atop of perovskite layer. Next, 30 nm of VOx was deposited atop the PTAA layer on the whole sample surface using the physical vapor deposition (PVD) technique. Silver electrodes (100 nm) were evaporated in a high vacuum (10-6 mbar) through a shadow mask, defining the active area of each device as ~0.16 cm2. The prepared samples (thin films and solar cells) were packed in Al lamination foil inside the argon glove box. The set of samples consisted of 6 thin films and 6 solar cells, which were exposed to 6, 10, and 21 kGy (2 samples per dose) with 137Cs gamma-ray source (E = 662 keV) with a dose rate of 2.5 Gy/min. The exposed samples will be studied on a focused ion beam (FIB) on a dual-beam scanning electron microscope from ThermoFisher, the Helios G4 Plasma FIB Uxe, operating with a xenon plasma.

Keywords: perovskite solar cells, transmission electron microscopy, radiation hardness, gamma irradiation

Procedia PDF Downloads 28

Authors: Kalaya Sribuddhachart, Mayuree Pumipaiboon, Mayuva Youngsabanant-Areekijseree

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The ultrastructure of 20 species of pheasant eggshells in Thailand, (Simese Fireback, Lophura diardi), (Silver Pheasant, Lophura nycthemera), (Kalij Pheasant, Lophura leucomelanos crawfurdii), (Kalij Pheasant, Lophura leucomelanos lineata), (Red Junglefowl, Gallus gallus spadiceus), (Crested Fireback, Lophura ignita rufa), (Green Peafowl, Pavo muticus), (Indian Peafowl, Pavo cristatus), (Grey Peacock Pheasant, Polyplectron bicalcaratum bicalcaratum), (Lesser Bornean Fireback, Lophura ignita ignita), (Green Junglefowl, Gallus varius), (Hume's Pheasant, Syrmaticus humiae humiae), (Himalayan Monal, Lophophorus impejanus), Golden Pheasant, Chrysolophus pictus, (Ring-Neck Pheasant, Phasianus sp.), (Reeves’s Pheasant, Syrmaticus reevesi), (Polish Chicken, Gallus sp.), (Brahma Chicken, Gallus sp.), (Yellow Golden Pheasant, Chrysolophus pictus luteus), and (Lady Amhersts Pheasant, Chrysolophus amherstiae) were studied by Secondary electron imaging (SEI) and Energy dispersive X-ray analysis (EDX) detectors of scanning electron microscope. Generally, all pheasant eggshells showed 3 layers of cuticle, palisade, and mammillary. The total thickness was ranging from 190.28±5.94-838.96±16.31µm. The palisade layer is the most thickness layer following by mammillary and cuticle layers. The palisade layer in all pheasant eggshells consisted of numerous vesicle holes that were firmly forming as network thorough the layer. The vesicle holes in all pheasant eggshells had difference porosity ranging from 0.44±0.11-0.23±0.05 µm. While the mammillary layer was the most compact layer with a variable shape (broad-base V and U-shape) connect to shell membrane. Elemental analysis by of 20 specie eggshells showed 9 apparent elements including carbon (C), oxygen (O), calcium (Ca), phosphorous (P), sulfur (S), magnesium (Mg), silicon (Si), aluminum (Al), and copper (Cu) at the percentage of 28.90- 8.33%, 60.64-27.61%, 55.30-14.49%, 1.97-0.03%, 0.08-0.03%, 0.50-0.16%, 0.30-0.04%, 0.06-0.02%, and 2.67-1.73%, respectively. It was found that Ca, C, and O showed highest elemental compositions, which essential for pheasant embryonic development, mainly presented as composited structure of calcium carbonate (CaCO3) more than 97%. Meanwhile, Mg, S, Si, Al, and P were major inorganic constituents of the eggshells which directly related to an increase of the shell hardness. Finally, the percentage of heavy metal copper (Cu) has been observed in 4 eggshell species. There are Golden Pheasant (2.67±0.16%), Indian Peafowl (2.61±0.13%), Green Peafowl (1.97±0.74%), and Silver Pheasant (1.73±0.11%), respectively. A non-significant difference was found in the percentages of 9 elements in all pheasant eggshells. This study is useful to provide the information of biology and taxonomic of pheasant study in Thailand for conservation.

Keywords: pheasants eggshells, secondary electron imaging (SEI) and energy dispersive X-ray analysis (EDX), morphology, Thailand

Procedia PDF Downloads 235

Authors: Pachari Chuenta, Suwat Nanan

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ZnO nanostructures have been synthesized successfully in high yield via catalyst-free chemical precipitation technique by varying zinc source (either zinc nitrate or zinc acetate) and oxygen source (either oxalic acid or urea) without using any surfactant, organic solvent or capping agent. The ZnO nanostructures were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffractometry (XRD), scanning electron microscopy (SEM), thermal gravimetric analysis (TGA), UV-vis diffuse reflection spectroscopy (UV-vis DRS), and photoluminescence spectroscopy (PL). The FTIR peak in the range of 450-470 cm-1 corresponded to Zn-O stretching in ZnO structure. The synthesized ZnO samples showed well crystalized hexagonal wurtzite structure. SEM micrographs displayed spherical droplet of about 50-100 nm. The band gap of prepared ZnO was found to be 3.4-3.5 eV. The presence of PL peak at 468 nm was attributed to surface defect state. The photocatalytic activity of ZnO was studied by monitoring the photodegradation of reactive red (RR141) azo dye under ultraviolet (UV) light irradiation. Blank experiment was also separately carried out by irradiating the aqueous solution of the dye in absence of the photocatalyst. The initial concentration of the dye was fixed at 10 mgL-1. About 50 mg of ZnO photocatalyst was dispersed in 200 mL dye solution. The sample was collected at a regular time interval during the irradiation and then was analyzed after centrifugation. The concentration of the dye was determined by monitoring the absorbance at its maximum wavelength (λₘₐₓ) of 544 nm using UV-vis spectroscopic analysis technique. The sources of Zn and O played an important role on photocatalytic performance of the ZnO photocatalyst. ZnO nanoparticles which prepared by zinc acetate and oxalic acid at molar ratio of 1:1 showed high photocatalytic performance of about 97% toward photodegradation of reactive red azo dye (RR141) under UV light irradiation for only 60 min. This work demonstrates the promising potential of ZnO nanomaterials as photocatalysts for environmental remediation.

Keywords: azo dye, chemical precipitation, photocatalytic, ZnO

Procedia PDF Downloads 144

Authors: Debajyoti Bose

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Chitosan has received much attention as a functional biopolymer for diverse applications, especially in pharmaceutics and medicine. Chitosan is a positively charged natural biodegradable and biocompatible polymer. It is a linear polysaccharide consisting of β-1,4 linked monomers of glucosamine and N-acetylglucosamine. Chitosan can be mainly obtained from fungal sources during large fermentation process. In this study,three different fungal strains Aspergillus niger NCIM 1045, Aspergillus oryzae NCIM 645 and Mucor indicus MTCC 3318 were used for the production of chitosan. The growth mediums were optimized for maximum fungal production. The produced chitosan was characterized by determining degree of deacetylation. Chitosan possesses one reactive amino at the C-2 position of the glucosamine residue, and these amines confer important functional properties to chitosan which can be exploited for biofabrication to generate various chemically modified derivatives and explore their potential for pharmaceutical field. Chitosan nanoparticles were prepared by ionic cross-linking with tripolyphosphate (TPP). The major effect on encapsulation and release of protein (e.g. enzyme diastase) in chitosan-TPP nanoparticles was investigated in order to control the loading and release efficiency. It was noted that the chitosan loading and releasing efficiency as a nanocapsule, obtained from different fungal sources was almost near to initial enzyme activity(12026 U/ml) with a negligible loss. This signify, chitosan can be used as a polymeric drug as well as active component or protein carrier material in dosage by design due to its appealing properties such as biocompatibility, biodegradability, low toxicity and relatively low production cost from abundant natural sources. Based upon these initial experiments, studies were also carried out on modification of chitosan based nanocapsules incorporated with physiologically important enzymes and nutraceuticals for target delivery.

Keywords: fungi, chitosan, enzyme, nanocapsule

Procedia PDF Downloads 504

Authors: Andrey V. Khromov, Antonida V. Makhotenko, Ekaterina A. Snigir, Svetlana S. Makarova, Natalia O. Kalinina, Valentin V. Makarov, Mikhail E. Taliansky

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Due to its simplicity, CRISPR/Cas9 has become widely used and capable of inducing mutations in the genes of organisms of various kingdoms. The aim of this work was to develop applications for the efficient modification of DNA coding sequences of phytoene desaturase (PDS), coilin and vacuolar invertase (Solanum tuberosum) genes, and to develop a new nanoparticles carrier efficient technology to deliver the CRISPR/Cas9 system for editing the plant genome. For each of the genes - coilin, PDS and vacuolar invertase, five single RNA guide (sgRNAs) were synthesized. To determine the most suitable nanoplatform, two types of NP platforms were used: magnetic NPs (MNPS) and gold NPs (AuNPs). To test the penetration efficiency, they were functionalized with fluorescent agents - BSA * FITS and GFP, as well as labeled Cy3 small-sized RNA. To measure the efficiency, a fluorescence and confocal microscopy were used. It was shown that the best of these options were AuNP - both in the case of proteins and in the case of RNA. The next step was to check the possibility of delivering components of the CRISPR/Cas9 system to plant cells for editing target genes. AuNPs were functionalized with a ribonucleoprotein complex consisting of Cas9 and corresponding to target genes sgRNAs, and they were biolistically bombarded to axillary buds and apical meristems of potato plants. After the treatment by the best NP carrier, potato meristems were grown to adult plants. DNA isolated from this plants was sent to a preliminary fragment of the analysis to screen out the non-transformed samples, and then to the NGS. The present work was carried out with the financial support from the Russian Science Foundation (grant No. 16-16-04019).

Keywords: biobombardment, coilin, CRISPR/Cas9, nanoparticles, NPs, PDS, sgRNA, vacuolar invertase

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Authors: M. Insiat Islam Rabby, M. Mahbubur Rahman, Eshanul Islam, A. K. M. Sadrul Islam

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The numerical and simulative analysis of laminar heat exchange convection of aluminum oxide (Al₂O₃) - water nanofluid for the developed region through two parallel plates is presented in this present work. The second order single phase energy equation, mass and momentum equation are solved by using finite volume method with the ANSYS FLUENT 16 software. The distance between two parallel plates is 4 mm and length is 600 mm. Aluminum oxide (Al₂O₃) is used as nanoparticle and water is used as the base/working fluid for the investigation. At the time of simulation 1% to 5% volume concentrations of the Al₂O₃ nanoparticles are used for mixing with water to produce nanofluid and a wide range of interval of Reynolds number from 500 to 1100 at constant heat flux 500 W/m² at the channel wall has also been introduced. The result reveals that for increasing the Reynolds number the Nusselt number and heat transfer coefficient are increased linearly and friction factor decreased linearly in the developed region for both water and Al₂O₃-H₂O nanofluid. By increasing the volume fraction of Al₂O₃-H₂O nanofluid from 1% to 5% the value of Nusselt number increased rapidly from 0.7 to 7.32%, heat transfer coefficient increased 7.14% to 31.5% and friction factor increased very little from 0.1% to 4% for constant Reynolds number compared to pure water. At constant heat transfer coefficient 700 W/m2-K the pumping power advantages have been achieved 20% for 1% volume concentration and 62% for 3% volume concentration of nanofluid compared to pure water.

Keywords: convective heat transfer, pumping power, constant heat flux, nanofluid, nanoparticles, volume concentration, thermal conductivity

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Authors: Hongquan Zhang

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Inspired by endogenous protein motors, researchers have constructed various synthetic DNA motors based on the specificity and predictability of Watson-Crick base pairing. However, the application of DNA motors to signal amplification and biosensing is limited because of low mobility and difficulty in real-time monitoring of the walking process. The objective of our work was to construct a new type of DNA motor termed target-triggered DNA motors that can walk for hundreds of steps in response to a single target binding event. To improve the mobility and processivity of DNA motors, we used gold nanoparticles (AuNPs) as scaffolds to build high-density, three-dimensional tracks. Hundreds of track strands are conjugated to a single AuNP. To enable DNA motors to respond to specific protein and nucleic acid targets, we adapted the binding-induced DNA assembly into the design of the target-triggered DNA motors. In response to the binding of specific target molecules, DNA motors are activated to autonomously walk along AuNP, which is powered by a nicking endonuclease or DNAzyme-catalyzed cleavage of track strands. Each moving step restores the fluorescence of a dye molecule, enabling monitoring of the operation of DNA motors in real time. The motors can translate a single binding event into the generation of hundreds of oligonucleotides from a single nanoparticle. The motors have been applied to amplify the detection of proteins and nucleic acids in test tubes and live cells. The motors were able to detect low pM concentrations of specific protein and nucleic acid targets in homogeneous solutions without the need for separation. Target-triggered DNA motors are significant for broadening applications of DNA motors to molecular sensing, cell imagining, molecular interaction monitoring, and controlled delivery and release of therapeutics.

Keywords: biosensing, DNA motors, gold nanoparticles, signal amplification

Procedia PDF Downloads 85

Authors: Oluwatoyin Joseph Gbadeyan, Sarp Adali, Bright Glen, Bruce Sithole

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Sodium lauryl surfactant concentration optimization, for nanoparticle production, provided the platform for advanced research studies. Different concentrations (0.05 %, 0.1 %, and 0.2 %) of sodium lauryl surfactant was added to snail shells powder during milling processes for producing CaCO3 at smaller particle size. Epoxy nanocomposites prepared at filler content 2 wt.% synthesized with different volumes of sodium lauryl surfactant were fabricated using a conventional resin casting method. Mechanical properties such as tensile strength, stiffness, and hardness of prepared nanocomposites was investigated to determine the effect of sodium lauryl surfactant concentration on nanocomposite properties. It was observed that the loading of the synthesized nano-calcium carbonate improved the mechanical properties of neat epoxy at lower concentrations of sodium lauryl surfactant 0.05 %. Meaningfully, loading of achatina fulica snail shell nanoparticles manufactures, with small concentrations of sodium lauryl surfactant 0.05 %, increased the neat epoxy tensile strength by 26%, stiffness by 55%, and hardness by 38%. Homogeneous dispersion facilitated, by the addition of sodium lauryl surfactant during milling processes, improved mechanical properties. Research evidence suggests that nano-CaCO3, synthesized from achatina fulica snail shell, possesses suitable reinforcement properties that can be used for nanocomposite fabrication. The evidence showed that adding small concentrations of sodium lauryl surfactant 0.05 %, improved dispersion of nanoparticles in polymetrix material that provided mechanical properties improvement.

Keywords: sodium lauryl surfactant, mechanical properties , achatina fulica snail shel, calcium carbonate nanopowder

Procedia PDF Downloads 148

Authors: Sira Suren, Soorathep Kheawhom

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This work focuses the development of thin and flexible zinc-air battery. The battery with an overall thickness of about 300 μm was fabricated by an inexpensive screen-printing technique. Commercial nano-silver ink was used as both current collectors and catalyst layer. Carbon black ink was used to fabricate cathode electrode. Polypropylene membrane was used as the cathode substrate and separator. 9 M KOH was used as the electrolyte. A mixture of Zn powder and ZnO was used to prepare the anode electrode. Types of conductive materials (Bi2O3, Na2O3Si and carbon black) for the anode and its concentration were investigated. Results showed that the battery using 29% carbon black showed the best performance. The open-circuit voltage and energy density observed were 1.6 V and 694 Wh/kg, respectively. When the battery was discharged at 10 mA/cm2, the potential voltage observed was 1.35 V. Furthermore, the battery was tested for its flexibility. Upon bending, no significant loss in performance was observed.

Keywords: flexible, Gel Electrolyte, screen printing, thin battery, Zn-Air battery

Procedia PDF Downloads 210

Authors: Yu. Mateyshina, A. Ulihin, N. Uvarov

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Supercapacitors are one of the most promising devices for energy storage applications as they can provide higher power density than batteries and higher energy density than conventional dielectric capacitors. Carbon materials with various microtextures are considered as main candidates for supercapacitors in terms of high surface area, interconnected pore structure, controlled pore size, high electrical conductivity and environmental friendliness. The specific capacitance (C) of the electrode material of the Electrochemical Double Layer Capacitors (EDLC) is known to depend on the specific surface area (Ss) and the pore structure. Activated carbons are most commonly used in supercapacitors because of their high surface area (Ss ≥ 1000 m2/g), good adhesion to electrolytes and low cost. In this work, electrochemical properties of new microporous and mesoporous carbon electrode materials were studied. The aim of the work was to investigate the relationship between the specific capacitance and specific surface area in a series of materials prepared from different organic precursors.. As supporting matrixes different carbon samples with Ss = 100-2000 m2/g were used. The materials were modified by treatment in acids (H2SO4, HNO3, acetic acid) in order to enable surface hydrophilicity. Then nanoparticles of transition metal oxides (for example NiO) were deposited on the carbon surfaces using methods of salts impregnation, mechanical treatment in ball mills and the precursors decomposition. The electrochemical characteristics of electrode hybrid materials were investigated in a symmetrical two-electrode cell using an impedance spectroscopy, voltammetry in both potentiodynamic and galvanostatic modes. It was shown that the value of C for the materials under study strongly depended on the preparation method of the electrode and the type of electrolyte (1 M H2SO4, 6 M KOH, 1 M LiClO4 in acetonitryl). Specific capacity may be increased by the introduction of nanoparticles from 50-100 F/g for initial carbon materials to 150-300 F/g for nanocomposites which may be used in supercapacitors. The work is supported by the по SC-14.604.21.0013.

Keywords: supercapacitors, carbon electrode, mesoporous carbon, electrochemistry

Procedia PDF Downloads 306

Authors: Kunwar Paritosh, Sanjay Mathur, Monika Yadav, Paras Gandhi, Subodh Kumar, Nidhi Pareek, Vivekanand Vivekanand

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A significant fraction of energy is wasted every year managing the biodegradable organic waste inadequately as development and sustainability are the inherent enemies. The management of these waste is indispensable to boost its optimum utilization by converting it to renewable energy resource (here biogas) through anaerobic digestion and to mitigate greenhouse gas emission. Food and yard wastes may prove to be appropriate and potential feedstocks for anaerobic co-digestion for biogas production. The present study has been performed to explore the synergistic effect of co-digesting food waste and yard trimmings from MNIT campus for enhanced biogas production in different ratios in batch tests (37±10C, 90 rpm, 45 days). The results were overwhelming and showed that blending two different organic waste in proper ratio improved the biogas generation considerably, with the highest biogas yield (2044±24 mLg-1VS) that was achieved at 75:25 of food waste to yard waste ratio on volatile solids (VS) basis. The yield was 1.7 and 2.2 folds higher than the mono-digestion of food or yard waste (1172±34, 1016±36mLg-1VS) respectively. The increase in biogas production may be credited to optimum C/N ratio resulting in higher yield. Also Adding TiO2 nanoparticles showed virtually no effect on biogas production as sometimes nanoparticles enhance biogas production. ICP-MS, FTIR analysis was carried out to gain an insight of feedstocks. Modified Gompertz and logistics models were applied for the kinetic study of biogas production where modified Gompertz model showed goodness-of-fit (R2=0.9978) with the experimental results.

Keywords: anaerobic co-digestion, biogas, kinetics, nanoparticle, organic waste

Procedia PDF Downloads 389

Authors: Marine Regnier, Pascal Bost, Matthieu Horgnies

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Some of the problems to be solved for the concrete industry are linked to the use of low-reactivity cement, the hardening of concrete under cold-weather and the manufacture of pre-casted concrete without costly heating step. The development of these applications needs to accelerate the hydration kinetics, in order to decrease the setting time and to obtain significant compressive strengths as soon as possible. The mechanisms enhancing the hydration kinetics of alite or Portland cement (e.g. the creation of nucleation sites) were already studied in literature (e.g. by using distinct additions such as titanium dioxide nanoparticles, calcium carbonate fillers, water-soluble polymers, C-S-H, etc.). However, the goal of this study was to establish a clear ranking of the efficiency of several types of additions by using a robust and reproducible methodology based on isothermal calorimetry (performed at 20°C). The cement was a CEM I 52.5N PM-ES (Blaine fineness of 455 m²/kg). To ensure the reproducibility of the experiments and avoid any decrease of the reactivity before use, the cement was stored in waterproof and sealed bags to avoid any contact with moisture and carbon dioxide. The experiments were performed on Portland cement pastes by using a water-to-cement ratio of 0.45, and incorporating different compounds (industrially available or laboratory-synthesized) that were selected according to their main composition and their specific surface area (SSA, calculated using the Brunauer-Emmett-Teller (BET) model and nitrogen adsorption isotherms performed at 77K). The intrinsic effects of (i) dry powders (e.g. fumed silica, activated charcoal, nano-precipitates of calcium carbonate, afwillite germs, nanoparticles of iron and iron oxides , etc.), and (ii) aqueous solutions (e.g. containing calcium chloride, hydrated Portland cement or Master X-SEED 100, etc.) were investigated. The influence of the amount of addition, calculated relatively to the dry extract of each addition compared to cement (and by conserving the same water-to-cement ratio) was also studied. The results demonstrated that the X-SEED®, the hydrated calcium nitrate, the calcium chloride (and, at a minor level, a solution of hydrated Portland cement) were able to accelerate the hydration kinetics of Portland cement, even at low concentration (e.g. 1%wt. of dry extract compared to cement). By using higher rates of additions, the fumed silica, the precipitated calcium carbonate and the titanium dioxide can also accelerate the hydration. In the case of the nano-precipitates of calcium carbonate, a correlation was established between the SSA and the accelerating effect. On the contrary, the nanoparticles of iron or iron oxides, the activated charcoal and the dried crystallised hydrates did not show any accelerating effect. Future experiments will be scheduled to establish the ranking of these additions, in terms of accelerating effect, by using low-reactivity cements and other water to cement ratios.

Keywords: acceleration, hydration kinetics, isothermal calorimetry, Portland cement

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Authors: Aniekan Peter, ECS Naidu, Edidiong Akang, U. Offor, R. Kalhapure, A. A. Chuturgoon, T. Govender, O. O. Azu

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Introduction: Nano-drugs are novel innovations in the management of human immunodeficiency virus (HIV) pandemic, especially resistant strains of the virus in their sanctuary sites: testis and the brain. There are safety concerns to be addressed to achieve the full potential of this new drug delivery system. Aim of study: Our study was designed to investigate toxicity profile of Tenofovir Nanoparticle (TDF-N) synthesized by University of Kwazulu-Natal (UKZN) Nano-team for prevention and treatment of HIV infection. Methodology: Ten adult male Sprague-Dawley rats maintained at the Animal House of the Biomedical Resources Unit UKZN were used for the study. The animals were weighed and divided into two groups of 5 animal each. Control animals (A) were administered with normal saline. Therapeutic dose (4.3 mg/kg) of TDF-N was administered to group B. At the end of four weeks, animals were weighed and sacrificed. Liver and kidney were removed fixed in formal saline, processed and stained using H/E, PAS and MT stains for light microscopy. Serum was obtained for renal function test (RFT), liver function test (LFT) and full blood count (FBC) using appropriate analysers. Cellular measurements were done using ImageJ and Leica software 2.0. Data were analysed using graph pad 6, values < 0.05 were significant. Results: We reported no histological alterations in the liver, kidney, FBC, LFT and RFT between the TDF-N animals and saline control. There were no significant differences in weight, organo-somatic index and histological measurements in the treatment group when compared with saline control. Conclusion/recommendations: TDF-N is not toxic to the liver, kidney and blood cells in our study. More studies using human subjects is recommended.

Keywords: tenofovir nanoparticles, liver, kidney, blood cells

Procedia PDF Downloads 185

Authors: Francisco Javier Montes Ruiz-Cabello, Guillermo Guerrero-Vacas, Sara Bermudez-Romero, Miguel Cabrerizo Vilchez, Miguel Angel Rodriguez-Valverde

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Galvanized steel is one of the widespread metallic materials used in industry. It consists on a iron-based alloy (steel) coated with a layer of zinc with variable thickness. The zinc is aimed to prevent the inner steel from corrosion and staining. Its production is cheaper than the stainless steel and this is the reason why it is employed in the construction of materials with large dimensions in aeronautics, urban/ industrial edification or ski-resorts. In all these applications, turning the natural hydrophilicity of the metal surface into superhydrophobicity is particularly interesting and would open a wide variety of additional functionalities. However, producing a superhydrophobic surface on galvanized steel may be a very difficult task. Superhydrophobic surfaces are characterized by a specific surface texture which is reached either by coating the surface with a material that incorporates such texture, or by conducting several roughening methods. Since galvanized steel is already a coated material, the incorporation of a second coating may be undesired. On the other hand, the methods that are recurrently used to incorporate the surface texture leading to superhydrophobicity in metals are aggressive and may damage their surface. In this work, we used a novel strategy which goal is to produce superhydrophobic galvanized steel by a two-step non-aggressive process. The first process is aimed to create a hierarchical structure by incorporating zinc nanoparticles sintered on the surface at a temperature slightly lower than the zinc’s melting point. The second one is a hydrophobization by a thick fluoropolymer layer deposition. The wettability of the samples is characterized in terms of tilting plate and bouncing drop experiments, while the roughness is analyzed by confocal microscopy. The durability of the produced surfaces was also explored.

Keywords: galvanaized steel, superhydrophobic surfaces, sintering nanoparticles, zinc nanopowder

Procedia PDF Downloads 151

Authors: M. Valentini, D. Melisi, M. A. Nitti, R A. Picca, M. C. Sportelli, E. Bonerba, G. Casamassima, N. Cioffi, L. Sabbatini, G. Tantillo, A. Valentini

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In recent years antimicrobial coatings are receiving increasing attention due to their high demand in medical applications as well as in healthcare and hygiene. Research and technology are constantly involved to develop advanced finishing which can provide bacteriostatic growth without compromising the other typical properties of a textile as durability and non-toxicity, just to cite a few. Here we report on the antimicrobial coatings obtained, at room temperature and without the use of solvents, by means of the ion beam co-sputtering technique of an Ag target and a polytetrafluoroethylene one. In particular, such method allows to conjugate the well-known antimicrobial action of silver with the anti-stain and water-repellent properties of the fluoropolymer. Moreover, different Ag nanoparticle loadings (φ) were prepared by tuning the material deposition conditions achieving a fine control on film thickness and their antimicrobial/anti-stain properties.

Keywords: antimicrobial, ion beam sputtering, nanocoatings, anti-stain

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Authors: Abdulmohsen Alruwaili

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A partial differential system featuring momentum and energy balance is often used to describe simulations of flow initiation and thermal shifting in boundary layers. The buoyancy force in terms of temperature is factored in the momentum balance equation. Buoyancy force causes the flow quantity to fluctuate along the streamwise direction 𝑋; therefore, the problem can be, to our best knowledge, analyzed through nonsimilar modeling. In this analysis, a nonsimilar model is evolved for radiative mixed convection of a magnetized power-law nanoliquid flow on top of a vertical plate installed in a stationary fluid. The upward linear stretching initiated the flow in the vertical direction. Assuming nanofluids are composite of copper (Cu) and alumina (Al₂O₃) nanoparticles, the viscous dissipation in this case is negligible. The nonsimilar system is dealt with analytically by local nonsimilarity (LNS) via numerical algorithm bvp4c. Surface temperature and flow field are shown visually in relation to factors like mixed convection, magnetic field strength, nanoparticle volume fraction, radiation parameters, and Prandtl number. The repercussions of magnetic and mixed convection parameters on the rate of energy transfer and friction coefficient are represented in tabular forms. The results obtained are compared to the published literature. It is found that the existence of nanoparticles significantly improves the temperature profile of considered nanoliquid. It is also observed that when the estimates of the magnetic parameter increase, the velocity profile decreases. Enhancement in nanoparticle concentration and mixed convection parameter improves the velocity profile.

Keywords: nanofluid, power law model, mixed convection, thermal radiation

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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

Procedia PDF Downloads 349

Authors: G. Wagner, R. Herrmann

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Cytotoxic platinum compounds play a major role in the chemotherapy of a large number of human cancers. However, due to the severe side effects for the patient and other problems associated with their use, there is a need for the development of more efficient drugs and new methods for their selective delivery to the tumours. One way to achieve the latter could be in the use of nanoparticular substrates that can adsorb or chemically bind the drug. In the cell, the drug is supposed to be slowly released, either by physical desorption or by dissolution of the particle framework. Ideally, the cytotoxic properties of the platinum drug unfold only then, in the cancer cell and over a longer period of time due to the gradual release. In this paper, we report on our first steps in this direction. The binding properties of a series of cytotoxic Pt(II) oxadiazoline compounds to mesoporous silica particles has been studied by NMR and UV/vis spectroscopy. High loadings were achieved when the Pt(II) compound was relatively polar, and has been dissolved in a relatively nonpolar solvent before the silica was added. Typically, 6-10 hours were required for complete equilibration, suggesting the adsorption did not only occur to the outer surface but also to the interior of the pores. The untreated and Pt(II) loaded particles were characterised by C, H, N combustion analysis, BET/BJH nitrogen sorption, electron microscopy (REM and TEM) and EDX. With the latter methods we were able to demonstrate the homogenous distribution of the Pt(II) compound on and in the silica particles, and no Pt(II) bulk precipitate had formed. The in vitro cytotoxicity in a human cancer cell line (HeLa) has been determined for one of the new platinum compounds adsorbed to mesoporous silica particles of different size, and compared with the corresponding compound in solution. The IC50 data are similar in all cases, suggesting that the release of the Pt(II) compound was relatively fast and possibly occurred before the particles reached the cells. Overall, the platinum drug is chemically stable on silica and retained its activity upon prolonged storage.

Keywords: cytotoxicity, mesoporous silica, nanoparticles, platinum compounds

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Authors: Luciana S. Almeida

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Nanotechnology has revolutionized the world of science and technology bringing great expectations due to its great potential of application in the most varied industrial sectors. The same characteristics that make nanoparticles interesting from the point of view of the technological application, these may be undesirable when released into the environment. The small size of nanoparticles facilitates their diffusion and transport in the atmosphere, water, and soil and facilitates the entry and accumulation of nanoparticles in living cells. The main objective of this study is to evaluate the environmental regulatory process of nanomaterials in the Brazilian scenario. Three specific objectives were outlined. The first is to carry out a global scientometric study, in a research platform, with the purpose of identifying the main lines of study of nanomaterials in the environmental area. The second is to verify how environmental agencies in other countries have been working on this issue by means of a bibliographic review. And the third is to carry out an assessment of the Brazilian Nanotechnology Draft Law 6741/2013 with the state environmental agencies. This last one has the aim of identifying the knowledge of the subject by the environmental agencies and necessary resources available in the country for the implementation of the Policy. A questionnaire will be used as a tool for this evaluation to identify the operational elements and build indicators through the Environment of Evaluation Application, a computational application developed for the development of questionnaires. At the end will be verified the need to propose changes in the Draft Law of the National Nanotechnology Policy. Initial studies, in relation to the first specific objective, have already identified that Brazil stands out in the production of scientific publications in the area of nanotechnology, although the minority is in studies focused on environmental impact studies. Regarding the general panorama of other countries, some findings have also been raised. The United States has included the nanoform of the substances in an existing program in the EPA (Environmental Protection Agency), the TSCA (Toxic Substances Control Act). The European Union issued a draft of a document amending Regulation 1907/2006 of the European Parliament and Council to cover the nanoform of substances. Both programs are based on the study and identification of environmental risks associated with nanomaterials taking into consideration the product life cycle. In relation to Brazil, regarding the third specific objective, it is notable that the country does not have any regulations applicable to nanostructures, although there is a Draft Law in progress. In this document, it is possible to identify some requirements related to the environment, such as environmental inspection and licensing; industrial waste management; notification of accidents and application of sanctions. However, it is not known if these requirements are sufficient for the prevention of environmental impacts and if national environmental agencies will know how to apply them correctly. This study intends to serve as a basis for future actions regarding environmental management applied to the use of nanotechnology in Brazil.

Keywords: environment; management; nanotecnology; politics

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Authors: Marian Mihalik, Kornel Csach, Martin Kovalik, Matúš Mihalik, Martina Kubovčíková, Maria Zentková, Martin Vavra, Vladimír Girman, Jaroslav Briančin, Marija Perovic, Marija Boškovic, Magdalena Fitta, Robert Pelka

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Current nanomaterials for use in biomedicine are based mainly on iron oxides and on present knowledge on magnetic nanostructures. Manganites can represent another material which can be used optionally. Manganites and their unique electronic properties have been extensively studied in the last decades not only due to fundamental interest but to possible applications of colossal magnetoresistance, magnetocaloric effect, and ferroelectric properties. It was found that the oxygen-reduction reaction on perovskite oxide is intimately connected with metal ion e.g., orbital occupation. The effect of oxygen deviation from the stoichiometric composition on crystal structure was studied very carefully by many authors on LaMnO₃. Depending on oxygen content, the crystal structure changes from orthorhombic one to rhombohedric for oxygen content 3.1. In the case of hole-doped manganites, the change from the orthorhombic crystal structure, which is typical for La1-xCaxMnO3 based manganites, to the rhombohedric crystal structure (La1-xMxMnO₃ where M = K, Ag, and Sr based materials) results in an enormous increase of the Curie temperature. In our paper, we study the effect of oxygen content on crystal structure, thermal, and magnetic properties (including magnetocaloric effect) of La1-xAgxMnO₃nano particle system. The content of oxygen in samples was tuned by heat treatment in different thermal regimes and in various environment (air, oxygen, argon). Water nanosuspensions based on La0.80Ag0.15MnO₃ magnetic particles with the Curie temperature of about 43oC were prepared by two different approaches. First, by using a laboratory circulation mill for milling of powder in the presence of sodium dodecyl sulphate (SDS) and subsequent centrifugation. Second nanosuspension was prepared using an agate bowl, etching in citric acid and HNO3, ultrasound homogeniser, centrifugation, and dextran 40 kDA or 15 kDA as surfactant. Electrostatic stabilisation obtained by the first approach did not offer long term kinetic and aggregation colloidal stability and was unable to compensate for attractive forces between particles under a magnetic field. By the second approach, we prepared suspension oversaturated by dextran 40 kDA for steric stabilisation, with evidence of the presence of superparamagnetic behaviour. Low concentration of nanoparticles and not ideal coverage of nanoparticles impacting the stability of ferrofluids was the disadvantage of this approach. Strong steric stabilisation was observable at alcaic conditions under pH = ~10. Application of dextran 15 kDA leads to relatively stable ferrofluid with pH around physiological conditions, but desegregation of powder by HNO₃ was not effective enough, and the average size of fragments was to large of about 150 nm, and we did not see any signature of superparamagnetic behaviour. The prepared ferrofluids were characterised by scanning and transition microscope method, thermogravimetry, magnetization, and AC susceptibility measurements. Specific Absorption Rate measurements were undertaken on powder as well on ferrofluids in order to estimate the potential application of La₀.₈₀Ag₀.₁₅MnO₃ magnetic particles based ferrofluid for hyperthermia. Our complex study contains an investigation of biocompatibility and potential biohazard of this material.

Keywords: manganites, magnetic nanoparticles, oxygen content, magnetic phase transition, magnetocaloric effect, ferrofluid, hyperthermia

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Authors: B. Merdas

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The Guelma region constitutes a vast geothermal field whose local geothermal gradient is very high. Indeed, various thermal and thermo sources emerging in the region, including some at relatively high temperatures. In the mio Pliocene Hammam N'bails, basin emerges a hot spring that leaves develop a thick series of thermal travertine linked to it. Near the thermal emergences has settled a very special mineralization antimony and zinc and lead. The results of analyses of the thermal waters of the source of Hammam N'bails and the associated travertine, show abnormal values in Pb, Sb, Zn, As, and other metals, demonstrating the genetic link between those waters and mineralization. Hammam N'bails mineralizations by their mineral assembling represented and their association with the hot springs, are very similar to epithermal deposits with precious metals (gold and silver) like Senator mine in Turkey or ‘Carlin-type’ in Nevada (USA).

Keywords: hot springs, mineralization; basement faults, Guelma, NE Algeria

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Authors: Vidula Shevade, B. J. Nagare, Sajeev Chacko

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First principles simulation, meaning density functional theory (DFT) calculations with plane waves and pseudopotential, has become a prized technique in condensed matter theory. Nanoparticles (NP) have been known to possess good catalytic activities, especially for molecules such as CO, O₂, etc. Among the metal NPs, Aluminium based NPs are also widely known for their catalytic properties. Aluminium metal is a lightweight, excellent electrical, and thermal abundant chemical element in the earth’s crust. Aluminium NPs, when added to solid rocket fuel, help improve the combustion speed and considerably increase combustion heat and combustion stability. Adding aluminium NPs into normal Al/Al₂O₃ powder improves the sintering processes of the ceramics, with high heat transfer performance, increased density, and enhanced thermal conductivity of the sinter. We used VASP and Gaussian 0₃ package to compute the geometries, electronic structure, and bonding properties of Al₁₂Ni as well as its interaction with O₂ and CO molecules. Several MD simulations were carried out using VASP at various temperatures from which hundreds of structures were optimized, leading to 24 unique structures. These structures were then further optimized through a Gaussian package. The lowest energy structure of Al₁₂Ni has been reported to be a singlet. However, through our extensive search, we found a triplet state to be lower in energy. In our structure, the Ni atom is found to be on the surface, which gives the non-zero magnetic moment. Incidentally, O2 and CO molecules are also triplet in nature, due to which the Al₁₂-Ni cluster is likely to facilitate the oxidation process of the CO molecule. Our results show that the most favourable site for the CO molecule is the Ni atom and that for the O₂ molecule is the Al atom that is nearest to the Ni atom. Al₁₂Ni-O₂ and Al₁₂-Ni-CO structures we extracted using VMD. Al₁₂Ni nanocluster, due to in triplet electronic structure configuration, indicates it to be a potential candidate as a catalyst for oxidation of CO molecules.

Keywords: catalyst, gaussian, nanoparticles, oxidation

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Authors: Hossein Anaraki-Ardakani, Tayebe Heidari-Rakati

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An environmentally benign protocol for the one-pot, three-component synthesis of Triazolo[1,2-a]indazole-1,3,8-trione derivatives by condensation of dimedone, urazole and aromatic aldehydes catalyzed by HClO4/SiO2 NPS as an ecofriendly catalyst with high catalytic activity and reusability at 100 ºC under solvent-free conditions is reported. The reaction proceeds to completion within 20-30 min in 77-86 % yield.

Keywords: one-pot reaction, dimedone, triazoloindazole, urazole

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Authors: C. Mendoza Ramírez, M. Gambús Ordaz, R. Mercado Ojeda.

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Chemical solutions flooding with surfactants, based on their property of reducing the interfacial tension between crude oil and water, is a potential application of chemical enhanced oil recovery (CEOR), however, the high-rate retention of surfactants associated with adsorption in the porous medium and the complexity of the mineralogical composition of the reservoir rock generates a limitation in the efficiency of displacement of crude oil. This study evaluates the effect of the concentration of a mixture of anionic-non-ionic surfactants with silica nanoparticles, in a rock sample composed of 25.14% clay minerals of the kaolinite, chlorite, halloysite and montmorillonite type, according to the results of X-Ray Diffraction analysis and Scanning Electron Spectrometry (XRD and SEM, respectively). The amount of the surfactant mixture adsorbed on the clay rock minerals was analyzed from the construction of its calibration curve and the 4-Region Isotherm Model in a UV-Visible spectroscopy. The adsorption rate of the surfactant in the clay rock averages 32% across all concentrations, influenced by the presence of the surface area of the substrate with a value of 1.6 m2/g and by the mineralogical composition of the clay that increases the cation exchange capacity (CEC). In addition, on Region I and II a final concentration measurement is not evident in the UV-VIS, due to its ionic nature, its high affinity with the clay rock and its low concentration. Finally, for potential CEOR applications, the adsorption of these mixed surfactant systems is considered due to their industrial relevance and it is concluded that it is possible to use concentrations in Region III and IV; initially the adsorption has an increasing slope and then reaches zero in the equilibrium where interfacial tension values are reached in the order of x10-1 mN/m.

Keywords: anionic–nonionic surfactants, clay rock, adsorption, 4-region isotherm model, cation exchange capacity, critical micelle concentration, enhanced oil recovery

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Authors: Qiong Tian, Lifeng Zhang, Demei Yu, Ajit D. Kelkar

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Low specific weight and high strength is the basic requirement for aerospace materials. Fiber-reinforced epoxy resin composites are attractive materials for this purpose. Boron nitride nanoparticles (BNNPs) have good radiation shielding capacity, which is very important to aerospace materials. Herein a processing route for an advanced hybrid composite material is demonstrated by introducing dispersed BNNPs in standard prepreg manufacturing. The hybrid materials contain three parts: E-fiberglass, an aerospace-grade epoxy resin system, and BNNPs. A vacuum assisted resin transfer molding (VARTM) was utilized in this processing. Two BNNP functionalization approaches are presented in this study: (a) covalent functionalization with 3-aminopropyltriethoxysilane (KH-550); (b) non-covalent functionalization with cetyltrimethylammonium bromide (CTAB). The functionalized BNNPs were characterized by Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction(XRD) and scanning electron microscope (SEM). The results showed that BN powder was successfully functionalized via the covalent and non-covalent approaches without any crystal structure change and big agglomerate particles were broken into platelet-like nanoparticles (BNNPs) after functionalization. Compared to pristine BN powder, surface modified BNNPs could result in significant improvement in mechanical properties such as tensile, flexural and compressive strength and modulus. CTAB functionalized BNNPs (CTAB-BNNPs) showed higher tensile and flexural strength but lower compressive strength than KH-550 functionalized BNNPs (KH550-BNNPs). These reinforcements are mainly attributed to good BNNPs dispersion and interfacial adhesion between epoxy matrix and BNNPs. This study reveals the potential in improving mechanical properties of BNNPs-containing composites laminates through surface functionalization of BNNPs.

Keywords: boron nitride, epoxy, functionalization, prepreg, composite

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Authors: Sneha Kumari, Ravi Krishnan Elangovan

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This abstract describes the development of a high-speed tracking method by modification in motor components for nanoparticle attachment. Myosin motors are nano-sized protein machines powering movement that defines life. These miniature molecular devices serve as engines utilizing chemical energy stored in ATP to produce useful mechanical energy in the form of a few nanometre displacement events leading to force generation that is required for cargo transport, cell division, cell locomotion, translated to macroscopic movements like running etc. With the advent of in vitro motility assay (IVMA), detailed functional studies of the actomyosin system could be performed. The major challenge with the currently available IVMA for tracking actin filaments is a resolution limitation of ± 50nm. To overcome this, we are trying to develop Single Molecule IVMA in which nanoparticle (GNP/QD) will be attached along or on the barbed end of actin filaments using CapZ protein and visualization by a compact TIRF module called ‘cTIRF’. The waveguide-based illumination by cTIRF offers a unique separation of excitation and collection optics, enabling imaging by scattering without emission filters. So, this technology is well equipped to perform tracking with high precision in temporal resolution of 2ms with significantly improved SNR by 100-fold as compared to conventional TIRF. Also, the nanoparticles (QD/GNP) attached to actin filament act as a point source of light coffering ease in filament tracking compared to conventional manual tracking. Moreover, the attachment of cargo (QD/GNP) to the thin filament paves the way for various nano-technological applications through their transportation to different predetermined locations on the chip

Keywords: actin, cargo, IVMA, myosin motors and single-molecule system

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Authors: Guadalupe Stefanny Aguilar-Moreno, Miguel Angel Aguilar-Mendez, Teodoro Espinosa-Solares

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In the agricultural sector, one of the main emitters of greenhouse gases is manure management, which has been increased considerably in recent years. Biogas is an energy source that can be produced from different organic materials through anaerobic digestion (AD); however, production efficiency is still low. Several techniques have been studied to increase its performance, such as co-digestion, the variation of digestion conditions, and nanomaterials used. Therefore, the aim of this investigation was to evaluate the effect of magnetite nanoparticles (NPs) concentration, synthesized by co-precipitation, on the biogas and methane production in AD using chicken litter as a substrate. Synthesis of NPs was performed according to the co-precipitation method, for which a fractional factorial experimental design 25⁻² with two replications was used. The study factors were concentrations (precursors and passivating), time of sonication and dissolution temperatures, and the response variables were size, hydrodynamic diameter (HD) and zeta potential. Subsequently, the treatment that presented the smallest NPs was chosen for their use on AD. The AD was established in serological bottles with a working volume of 250 mL, incubated at 36 ± 1 °C for 80 days. The treatments consisted of the addition of different concentrations of NPs in the microcosms: chicken litter only (control), 20 mg∙L⁻¹ of NPs + chicken litter, 40 mg∙L⁻¹ of NPs + chicken litter and 60 mg∙L⁻¹ of NPs + chicken litter, all by triplicate. Methane and biogas production were evaluated daily. The smallest HD (49.5 nm) and the most stable NPs (21.22 mV) were obtained with the highest passivating concentration and the lower precursors dissolution temperature, which were the only factors that had a significant effect on the HD. In the transmission electron microscopy performed to these NPs, an average size of 4.2 ± 0.73 nm was observed. The highest biogas and methane production was obtained with the treatment that had 20 mg∙L⁻¹ of NPs, being 29.5 and 73.9%, respectively, higher than the control, while the treatment with the highest concentration of NPs was not statistically different from the control. From the above, it can be concluded that the magnetite NPs promote the biogas and methane production in AD; however, high concentrations may cause inhibitory effects among methanogenic microorganisms.

Keywords: agricultural sector, anaerobic digestion, nanotechnology, waste management

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Authors: Dorottya Guban, Irina Borbath, Istvan Bakos, Peter Nemeth, Andras Tompos

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One of the greatest challenges of the implementation of polymer electrolyte membrane fuel cells (PEMFCs) is to find active and durable electrocatalysts. The cell performance is always limited by the oxygen reduction reaction (ORR) on the cathode since it is at least 6 orders of magnitude slower than the hydrogen oxidation on the anode. Therefore high loading of Pt is required. Catalyst corrosion is also more significant on the cathode, especially in case of mobile applications, where rapid changes of loading have to be tolerated. Pt-Sn bulk alloys and SnO2-decorated Pt3Sn nanostructures are among the most studied bimetallic systems for fuel cell applications. Exclusive formation of supported Sn-Pt alloy phases with different Pt/Sn ratios can be achieved by using controlled surface reactions (CSRs) between hydrogen adsorbed on Pt sites and tetraethyl tin. In this contribution our results for commercial and a home-made 20 wt.% Pt/C catalysts modified by tin anchoring via CSRs are presented. The parent Pt/C catalysts were synthesized by modified NaBH4-assisted ethylene-glycol reduction method using ethanol as a solvent, which resulted either in dispersed and highly stable Pt nanoparticles or evenly distributed raspberry-like agglomerates according to the chosen synthesis parameters. The 20 wt.% Pt/C catalysts prepared that way showed improved electrocatalytic performance in the ORR and stability in comparison to the commercial 20 wt.% Pt/C catalysts. Then, in order to obtain Sn-Pt/C catalysts with Pt/Sn= 3 ratio, the Pt/C catalysts were modified with tetraethyl tin (SnEt4) using three and five consecutive tin anchoring periods. According to in situ XPS studies in case of catalysts with highly dispersed Pt nanoparticles, pre-treatment in hydrogen even at 170°C resulted in complete reduction of the ionic tin to Sn0. No evidence of the presence of SnO2 phase was found by means of the XRD and EDS analysis. These results demonstrate that the method of CSRs is a powerful tool to create Pt-Sn bimetallic nanoparticles exclusively, without tin deposition onto the carbon support. On the contrary, the XPS results revealed that the tin-modified catalysts with raspberry-like Pt agglomerates always contained a fraction of non-reducible tin oxide. At the same time, they showed increased activity and long-term stability in the ORR than Pt/C, which was assigned to the presence of SnO2 in close proximity/contact with Pt-Sn alloy phase. It has been demonstrated that the content and dispersion of the fcc Pt3Sn phase within the electrocatalysts can be controlled by tuning the reaction conditions of CSRs. The bimetallic catalysts displayed an outstanding performance in the ORR. The preparation of a highly dispersed 20Pt/C catalyst permits to decrease the Pt content without relevant decline in the electrocatalytic performance of the catalysts.

Keywords: anode catalyst, cathode catalyst, controlled surface reactions, oxygen reduction reaction, PtSn/C electrocatalyst

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Authors: Reza Vakili, Xiaolei Fan, Alex Walton

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The first near ambient pressure (NAP)-XPS study of CO oxidation over Pt nanoparticles (NPs) incorporated into Zr-based UiO (UiO for Universitetet i Oslo) MOFs was carried out. For this purpose, the MOF-based Catalysts were prepared by wetness impregnation (WI-PtNPs@UiO-67) and linker design (LD-PtNPs@UiO-67) methods along with PtNPs@ZrO₂ as the control catalyst. Firstly, the as-synthesized catalysts were reduced in situ prior to the operando XPS analysis. The existence of Pt(II) species was proved in UiO-67 by observing Pt 4f core level peaks at a high binding energy of 72.6 ± 0.1 eV. However, by heating the WI-PtNPs@UiO-67 catalyst in situ to 200 °C under vacuum, the higher BE components disappear, leaving only the metallic Pt 4f doublet, confirming the formation of Pt NPs. The complete reduction of LD-PtNPs@UiO-67 is achieved at 250 °C and 1 mbar H₂. To understand the chemical state of Pt NPs in UiO-67 during catalytic turnover, we analyzed the Pt 4f region using operando NAP-XPS in the temperature-programmed measurements (100-260 °C) with reference to PtNPs@ZrO₂ catalyst. CO conversion during NAP-XPS experiments with the stoichiometric mixture shows that LD-PtNPs@UiO-67 has a better CO turnover frequency (TOF, 0.066 s⁻¹ at 260 °C) than the other two (ca. 0.055 s⁻¹). Pt 4f peaks only show one chemical species present at all temperatures, but the core level BE shifts change as a function of reaction temperature, i.e., Pt 4f peak from 71.8 eV at T < 200 °C to 71.2 eV at T > 200 °C. As this higher BE state of 71.8 eV was not observed after in situ reductions of the catalysts and only once the CO/O₂ mixture was introduced, we attribute it to the surface saturation of Pt NPs with adsorbed CO. In general, the quantitative analysis of Pt 4f data from the operando NAP-XPS experiments shows that the surface chemistry of the Pt active phase in the two PtNPs@UiO-67 catalysts is the same, comparable to that of PtNPs@ZrO₂. The observed difference in the catalytic activity can be attributed to the particle sizes of Pt NPs, as well as the dispersion of active phase in the support, which are different in the three catalysts.

Keywords: CO oxidation, heterogeneous catalysis, MOFs, Metal Organic Frameworks, NAP-XPS, Near Ambient Pressure X-ray Photoelectron Spectroscopy

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Authors: Weiam Daear, Patrick Lai, Elmar Prenner

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The human body offers many avenues that could be used for drug delivery. The pulmonary route, which is delivered through the lungs, presents many advantages that have sparked interested in the field. These advantages include; 1) direct access to the lungs and the large surface area it provides, and 2) close proximity to the blood circulation. The air-blood barrier of the alveoli is about 500 nm thick. The air-blood barrier consist of a monolayer of lipids and few proteins called the lung surfactant and cells. This monolayer consists of ~90% lipids and ~10% proteins that are produced by the alveolar epithelial cells. The two major lipid classes constitutes of various saturation and chain length of phosphatidylcholine (PC) and phosphatidylglycerol (PG) representing 80% of total lipid component. The major role of the lung surfactant monolayer is to reduce surface tension experienced during breathing cycles in order to prevent lung collapse. In terms of the pulmonary drug delivery route, drugs pass through various parts of the respiratory system before reaching the alveoli. It is at this location that the lung surfactant functions as the air-blood barrier for drugs. As the field of nanomedicine advances, the use of nanoparticles (NPs) as drug delivery vehicles is becoming very important. This is due to the advantages NPs provide with their large surface area and potential specific targeting. Therefore, studying the interaction of NPs with lung surfactant and whether they affect its stability becomes very essential. The aim of this research is to develop a biomimetic model of the human lung surfactant followed by a biophysical analysis of the interaction of polymeric NPs. This biomimetic model will function as a fast initial mode of testing for whether NPs affect the stability of the human lung surfactant. The model developed thus far is an 8-component lipid system that contains major PC and PG lipids. Recently, a custom made 16:0/16:1 PC and PG lipids were added to the model system. In the human lung surfactant, these lipids constitute 16% of the total lipid component. According to the author’s knowledge, there is not much monolayer data on the biophysical analysis of the 16:0/16:1 lipids, therefore more analysis will be discussed here. Biophysical techniques such as the Langmuir Trough is used for stability measurements which monitors changes to a monolayer's surface pressure upon NP interaction. Furthermore, Brewster Angle Microscopy (BAM) employed to visualize changes to the lateral domain organization. Results show preferential interactions of NPs with different lipid groups that is also dependent on the monolayer fluidity. Furthermore, results show that the film stability upon compression is unaffected, but there are significant changes in the lateral domain organization of the lung surfactant upon NP addition. This research is significant in the field of pulmonary drug delivery. It is shown that NPs within a certain size range are safe for the pulmonary route, but little is known about the mode of interaction of those polymeric NPs. Moreover, this work will provide additional information about the nanotoxicology of NPs tested.

Keywords: Brewster angle microscopy, lipids, lung surfactant, nanoparticles

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