Search results for: superparamagnetic iron oxide nanoparticles (SPIONS)

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

Procedia PDF Downloads 321

Authors: J. D. Marinaccio, I. Mabbett, C. Glover, D. Worsley

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Through use of novel modern/rapid processing techniques such as screen printing and Near-Infrared (NIR) radiative curing, process time for the sintering of sintered nickel plaques, applicable to alkaline nickel battery chemistries, has been drastically reduced from in excess of 200 minutes with conventional convection methods to below 2 minutes using NIR curing methods. Steps have also been taken to remove the need for forming gas as a reducing agent by implementing carbon as an in-situ reducing agent, within the ink formulation.

Keywords: batteries, energy, iron, nickel, storage

Procedia PDF Downloads 441

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

Procedia PDF Downloads 123

Authors: Usman B.M., Basheer O. B., . Ahmed A., Amali N. U., Taufeeq O.

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This study presents an investigation into the improvement of strength properties of concrete using egg shell powder (ESP) and groundnut husk ash (GHA) as additives so as to reduce its high cost and find alternative disposal method for agricultural waste. A standard consistency test was carried out on the egg shell powder and groundnut husk ash. A prescribed concrete mix ratio of 1:2:4 concrete cubes (150mm by 150mm) and water-cement ratio of 0.6 were casted. A total of One hundred and forty four (144) cubes were cast and cured for 3, 7 and 28 days and compressive strength subsequently determined in comparison with the relevant specifications. Consistency test on the cement paste at the various concentrations exhibited an increase in the setting time as the concentration increases with the highest value recorded at 5% egg shell powder and groundnut husk ash concentration as 219 minutes for the initial setting time and 275 minutes for the final setting time as against the control specimen of 159 minutes and 234 minutes for both initial and final setting times respectively. The results of the investigations showed that GHA was predominantly of Silicon oxide (56.73%) and a combined SiO₂, Al₂O₃ and Fe₂O₃ content of 66.75%; and the result of the investigations showed that ESP was predominantly of Calcium oxide (52.75%) and a combined SiO₂, Al₂O₃ and Fe₂O₃ content of 3.86%. The addition of GHA and ESP in concrete showed slight different in compressive strength with increase in GHA and ESP additive up to 5% and high decrease in compressive strength with further increase in GHA and ESP content. The 28 days compressive strength of the concrete cubes; compared with that of the control; showed a slight increase. Thus the use of GHA and ESP as partial replacement of cement will provide an economic use of by-product and consequently produce a cheaper concrete construction without comprising its strength

Keywords: additive, concrete, eggshell powder, groundnut husk ash compressive strength

Procedia PDF Downloads 140

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: Laura Gonzalez, Santiago Benavides, Martha Elena Londono, Ana Elisa Casas, Adriana Restrepo-Osorio

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Cotton products are sensitive to microorganisms due to its ability to retain moisture, which might cause change into the coloration, mechanical properties reduction or foul odor generation; consequently, this represents risks to the health of users. Nowadays, have been carried out researches to give antibacterial properties to textiles using different strategies, which included the use of silver nanoparticles (AgNPs). The antibacterial behavior can be affected by laundering process reducing its effectiveness. In the other way, the environmental impact generated for the synthetic antibacterial agents has motivated to seek new and more ecological ways for produce AgNPs. The aims of this work are to determine the antibacterial activity of cotton fabric functionalized with green (G) and commercial (C) AgNPs after twenty washing cycles, also to evaluate morphological and color changes. A plain weave cotton fabric suitable for dyeing and two AgNPs solutions were use. C a commercial product and G produced using an ecological method, both solutions with 0.5 mM concentration were impregnated on cotton fabric without stabilizer, at a liquor to fabric ratio of 1:20 in constant agitation during 30min and then dried at 70 °C by 10 min. After that the samples were subjected to twenty washing cycles using phosphate-free detergent simulated on agitated flask at 150 rpm, then were centrifuged and dried on a tumble. The samples were characterized using Kirby-Bauer test determine antibacterial activity against E. coli y S. aureus microorganisms, the results were registered by photographs establishing the inhibition halo before and after the washing cycles, the tests were conducted in triplicate. Scanning electron microscope (SEM) was used to observe the morphologies of cotton fabric and treated samples. The color changes of cotton fabrics in relation to the untreated samples were obtained by spectrophotometer analysis. The images, reveals the presence of inhibition halo in the samples treated with C and G AgNPs solutions, even after twenty washing cycles, which indicated a good antibacterial activity and washing durability, with a tendency to better results against to S. aureus bacteria. The presence of AgNPs on the surface of cotton fiber and morphological changes were observed through SEM, after and before washing cycles. The own color of the cotton fiber has been significantly altered with both antibacterial solutions. According to the colorimetric results, the samples treated with C lead to yellowing while the samples modified with G to red yellowing Cotton fabrics treated AgNPs C and G from 0.5 mM solutions exhibited excellent antimicrobial activity against E. coli and S. aureus with good laundering durability effects. The surface of the cotton fibers was modified with the presence of AgNPs C and G due to the presence of NPs and its agglomerates. There are significant changes in the natural color of cotton fabric due to deposition of AgNPs C and G which were maintained after laundering process.

Keywords: antibacterial property, cotton fabric, fastness to wash, Kirby-Bauer test, silver nanoparticles

Procedia PDF Downloads 247

Authors: Nour S. Abdelrahman, Seunghyun Hong, Hassan A. Arafat, Daniel Choi, Faisal Al Marzooqi

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Abstract—The advancement of lithium extraction methods from water sources, particularly saltwater brine, is gaining prominence in the lithium recovery industry due to its cost-effectiveness. Traditional techniques like recrystallization, chemical precipitation, and solvent extraction for metal recovery from seawater or brine are energy-intensive and exhibit low efficiency. Moreover, the extensive use of organic solvents poses environmental concerns. As a result, there's a growing demand for environmentally friendly lithium recovery methods. Membrane-based separation technology has emerged as a promising alternative, offering high energy efficiency and ease of continuous operation. In our study, we explored the potential of lithium-selective sieve channels constructed from layers of 2D graphene oxide and MXene (transition metal carbides and nitrides), integrated with surface – SO₃₋ groups. The arrangement of these 2D sheets creates interplanar spacing ranging from 0.3 to 0.8 nm, which forms a barrier against multivalent ions while facilitating lithium-ion movement through nano capillaries. The introduction of the sulfonate group provides an effective pathway for Li⁺ ions, with a calculated binding energy of Li⁺ – SO³⁻ at – 0.77 eV, the lowest among monovalent species. These modified membranes demonstrated remarkably rapid transport of Li⁺ ions, efficiently distinguishing them from other monovalent and divalent species. This selectivity is achieved through a combination of size exclusion and varying binding affinities. The graphene oxide channels in these membranes showed exceptional inter-cation selectivity, with a Li⁺/Mg²⁺ selectivity ratio exceeding 104, surpassing commercial membranes. Additionally, these membranes achieved over 94% rejection of MgCl₂.

Keywords: ion permeation, lithium extraction, membrane-based separation, nanotechnology

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Authors: C. D’Urso, L. Frusteri, M. Samperi, G. Leonardi

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Solid metal halides are used as active cathode ingredients in the case of Na-NiCl2 batteries that require a fused secondary electrolyte, sodium tetrachloraluminate (NaAlCl4), to facilitate the movement of the Na+ ion into the cathode. The sodium-nickel chloride (Na - NiCl2) battery has been extensively investigated as a promising system for large-scale energy storage applications. The growth of Ni and NaCl particles in the cathodes is one of the most important factors that degrade the performance of the Na-NiCl2 battery. The larger the particles of active ingredients contained in the cathode, the smaller the active surface available for the electrochemical reaction. Therefore, the growth of Ni and NaCl particles can lead to an increase in cell polarization resulting from the reduced active area. A higher current density, a higher state of charge (SOC) at the end of the charge (EOC) and a lower Ni / NaCl ratio are the main parameters that result in the rapid growth of Ni particles. In light of these problems, cathode and chemistry Nano-materials with recognized and well-documented electrochemical functions have been studied and manufactured to simultaneously improve battery performance and develop less expensive and more performing, sustainable and environmentally friendly materials. Starting from the well-known cathodic material (Na-NiCl2), the new electrolytic materials have been prepared on the replacement of nickel with iron (10-90%substitution of Nichel with Iron), to obtain a new material with potential advantages compared to current battery technologies; for example,, (1) lower cost of cathode material compared to state of the art as well as (2) choices of cheaper materials (stainless steels could be used for cell components, including cathode current collectors and cell housings). The study on the particle size of the cathode and the physicochemical characterization of the cathode was carried out in the test cell using, where possible, the GITT method (galvanostatic technique of intermittent titration). Furthermore, the impact of temperature on the different cathode compositions of the positive electrode was studied. Especially the optimum operating temperature is an important parameter of the active material.

Keywords: critical raw materials, energy storage, sodium metal halide, battery

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Authors: Gadanya, A.M., Ponfa, S., Jibril, M.M., Abubakar, S. M.

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Background: Edible insects such as grasshopper are important sources of food for humans, and have been consumed as traditional foods by many indigenous communities especially in Africa, Asia, and Latin America. These communities have developed their skills and techniques in harvesting, preparing, consuming, and preserving edible insects, widely contributing to the role played by the use of insects in human nutrition. Aim/ objective: This study was aimed at determining the effect of insect enriched sprouted soyabean /millet based food on some gut health markers in albino rats. Methods. Four different formulations of Complementary foods (i.e Complementary Food B (CFB): sprouted millet (SM), Complementary Food C (CFC): sprouted soyabean (SSB), Complementary Food D (CFD): sprouted soybean and millet (SSBM) in a ratio of (50:50) and Complementary Food E (CFE): insect (grasshopper) enriched sprouted soybean and millet (SSBMI) in a ratio of (50:25:25)) were prepared. Proximate composition and short chain fatty acid contents were determined. Thirty albino rats were divided into5 groups of six rats each. Group 1(CDA) were fed with basal diet and served as a control group, while groups 2,3,4 and 5 were fed with the corresponding complimentary foods CFB, CFC, CFD and CFE respectively daily for four weeks. Concentrations of fecal protein, serum total carotenoids and nitric oxide were determined. DNA extraction for molecular isolation and characterization were carried out followed by PCR, the use of mega 11 software and NCBI blast for construction of the phylogenetic tree and organism identification respectively. Results: Significant increase (P<0.05) in percentage ash, fat, protein and moisture contents, as well as short chain fatty acid (acetate, butyrate and propionate) concentrations were recorded in the insect enriched sprouted composite food (CFE) when compared with the CFA, CFB, CFC and CFD composite food. Faecal protein, carotenoid and nitric oxide concentrations were significantly lower (P>0.05) in group 5 in comparison to groups 1to 4. Ruminococcus bromii and Bacteroidetes were molecularly isolated and characterized by 16s rRNA from the sprouted millet/sprouted soybean and the insect enriched sprouted soybean/sprouted millet based food respectively. The presence of these bacterial strains in the feaces of the treated rats is an indication that the gut of the treated rats is colonized by good gut bacteria, hence, an improved gut health. Conclusion: Insect enriched sprouted soya bean/sprouted millet based complementary diet showed a high composition of ash, fat, protein and fiber. Thus, could increase the availability of short chain fatty acids whose role to the host organism cannot be overemphasized. It was also found to have decrease the level of faecal protein, carotenoid and nitric oxide in the serum which is an indication of an improvement in the immune system function.

Keywords: gut-health, insect, millet, soybean, sprouted

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Authors: Bedarnia Ishak

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In the recent years, the dry reforming of methane has received considerable attention from an environmental view point because it consumes and eliminates two gases (CH4 and CO2) responsible for global warming by greenhouse effect. Many catalysts containing noble metal (Rh, Ru, Pd, Pt and Ir) or transition metal (Ni, Co and Fe) have been reported to be active in this reaction. Compared to noble metals, Ni-materials are cheap but very easily deactivated by coking. Ni-based mixed oxides structurally well-defined like perovskites and spinels are being studied because they possibly make solid solutions and allow to vary the composition and thus the performances properties. In this work, nano-sized nickel ferrite oxides are synthesized using three different methods: Co-precipitation (CP), hydrothermal (HT) and sol gel (SG) methods and characterized by XRD, Raman, XPS, BET, TPR, SEM-EDX and TEM-EDX. XRD patterns of all synthesized oxides showed the presence of NiFe2O4 spinel, confirmed by Raman spectroscopy. Hematite was present only in CP sample. Depending on the synthesis method, the surface area, particle size, as well as the surface Ni/Fe atomic ratio (XPS) and the behavior upon reduction varied. The materials were tested in methane dry reforming with CO2 at 1 atm and 650-800 °C. The catalytic activity of the spinel samples was not very high (XCH4 = 5-20 mol% and XCO2 = 25-40 mol %) when no pre-reduction step was carried out. A significant contribution of RWGS explained the low values of H2/CO ratio obtained. The reoxidation step of the catalyst carried out after reaction showed little amounts of coke deposition. The reducing pretreatment was particularly efficient in the case of SG (XCH4 = 80 mol% and XCO2 = 92 mol%, at 800 °C), with H2/CO > 1. In conclusion, the influence of preparation was strong for most samples and the catalytic behavior could be interpreted by considering the distribution of cations among octahedral (Oh) and tetrahedral (Td) sites as in (Ni2+1-xFe3+x) Td (Ni2+xFe3+2-x) OhO2-4 influenced the reducibility of materials and thus their catalytic performance.

Keywords: NiFe2O4, dry reforming of methane, spinel oxide, oxide zenc

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Authors: Sanjeev Singh

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Background: Obstructed total anomalous pulmonary venous connection (OTAPVC) typically presents with severe cardiovascular decompensation and requires urgent surgical management. Pulmonary arterial hypertension (PAH) is a major risk factor affecting mortality. Perioperative management focuses on providing inotropic support and managing potential pulmonary hypertensive episodes. The aim of this study was to determine the outcome of patients with high pulmonary arterial pressure (PAP) with milrinone alone and a combination of milrinone and inhaled nitric oxide (INO). Material and Methods: After the approval of the ethical committee, this single-center prospective randomized and observational study was conducted over a period of two years among eighty-six patients with obstructed TAPVC repair with severe PAH. Group-I patients received milrinone, and Group-II patients received both milrinone (after aortic cross-clamp removal) and INO during the post-operative period at the cardiac care unit (CCU). Clinical outcomes such as ventilation time, length of stay (LOS) in the CCU, LOS in the hospital, complications, and hospital mortality were compared between the two groups. Result: The average ventilation time, LOS in CCU, and LOS in hospital for group I were 96.82 ± 19.46 hours, 10.91 ± 7.53 days, and 14.46 ± 7.58 days, respectively, and for group II, it was 85.14 ± 15.79 hours, 7.28 ± 3.68 days, and 10.21 ± 3.14 days, respectively, which was statistically significantly lower for group II. Reintubation, RV dysfunction, and hospital mortality were 16.3%, 37.2%, and 6.9% in group I, and 4.8%, 14.6%, and 2.4% in group II, respectively. The P value for each variable was significant < 0.05 (except mortality). Conclusion: Preoperative obstruction is a risk factor for postoperative obstruction, as 235 patients with obstructed TAPVC had severe PAH (39.98%) in this study. Management of severe PAH with a combination of milrinone and INO had a better outcome than milrinone alone.

Keywords: inhaled nitric oxide, milrinone, pulmonary artery hypertension, total anomalous pulmonary venous connection

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Authors: Ligang Wang, Theodoros Damartzis, Stefan Diethelm, Jan Van Herle, François Marechal

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Biogas production from anaerobic digestion of organic sludge from wastewater treatment as well as various urban and agricultural organic wastes is of great significance to achieve a sustainable society. Two upgrading approaches for cleaned biogas can be considered: (1) direct H₂ injection for catalytic CO₂ methanation and (2) CO₂ separation from biogas. The first approach usually employs electrolysis technologies to generate hydrogen and increases the biogas production rate; while the second one usually applies commercially-available highly-selective membrane technologies to efficiently extract CO₂ from the biogas with the latter being then sent afterward for compression and storage for further use. A straightforward way of utilizing the captured CO₂ is on-site catalytic CO₂ methanation. From the perspective of system complexity, the second approach may be questioned, since it introduces an additional expensive membrane component for producing the same amount of methane. However, given the circumstance that the sustainability of the produced biogas should be retained after biogas upgrading, renewable electricity should be supplied to drive the electrolyzer. Therefore, considering the intermittent nature and seasonal variation of renewable electricity supply, the second approach offers high operational flexibility. This indicates that these two approaches should be compared based on the availability and scale of the local renewable power supply and not only the technical systems themselves. Solid-oxide electrolysis generally offers high overall system efficiency, and more importantly, it can achieve simultaneous electrolysis of CO₂ and H₂O (namely, co-electrolysis), which may bring significant benefits for the case of CO₂ separation from the produced biogas. When taking co-electrolysis into account, two additional upgrading approaches can be proposed: (1) direct steam injection into the biogas with the mixture going through the SOE, and (2) CO₂ separation from biogas which can be used later for co-electrolysis. The case study of integrating SOE to a wastewater treatment plant is investigated with wind power as the renewable power. The dynamic production of biogas is provided on an hourly basis with the corresponding oxygen and heating requirements. All four approaches mentioned above are investigated and compared thermo-economically: (a) steam-electrolysis with grid power, as the base case for steam electrolysis, (b) CO₂ separation and co-electrolysis with grid power, as the base case for co-electrolysis, (c) steam-electrolysis and CO₂ separation (and storage) with wind power, and (d) co-electrolysis and CO₂ separation (and storage) with wind power. The influence of the scale of wind power supply is investigated by a sensitivity analysis. The results derived provide general understanding on the economic competitiveness of SOE for sustainable biogas upgrading, thus assisting the decision making for biogas production sites. The research leading to the presented work is funded by European Union’s Horizon 2020 under grant agreements n° 699892 (ECo, topic H2020-JTI-FCH-2015-1) and SCCER BIOSWEET.

Keywords: biogas upgrading, solid-oxide electrolyzer, co-electrolysis, CO₂ utilization, energy storage

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Authors: Nikolai A. Khlebnikov, Vladimir N. Krasilnikov, Evgenii V. Polyakov, Anastasia A. Maltceva

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Carbon materials with advanced surfaces are widely used both in modern industry and in environmental protection. The physical-chemical nature of these materials is determined by the morphology of primary atomic and molecular carbon structures, which are the basis for synthesizing the following materials: zero-dimensional (fullerenes), one-dimensional (fiber, tubes), two-dimensional (graphene) carbon nanostructures, three-dimensional (multi-layer graphene, graphite, foams) with unique physical-chemical and functional properties. Experience shows that the microscopic morphological level is the basis for the creation of the next mesoscopic morphological level. The dependence of the morphology on the chemical way and process prehistory (crystallization, colloids formation, liquid crystal state and other) is the peculiarity of the last called level. These factors determine the consumer properties of carbon materials, such as specific surface area, porosity, chemical resistance in corrosive environments, catalytic and adsorption activities. Based on the developed ideology of thin precursor synthesis, the authors discuss one of the approaches of the porosity control of carbon-containing materials with a given aggregates morphology. The low-temperature thermolysis of precursors in a gas environment of a given composition is the basis of the above-mentioned idea. The processes of carbothermic precursor synthesis of two different compounds: tungsten carbide WC:nC and zinc oxide ZnO:nC containing an impurity phase in the form of free carbon were selected as subjects of the research. In the first case, the transition metal (tungsten) forming carbides was the object of the synthesis. In the second case, there was selected zinc that does not form carbides. The synthesis of both kinds of transition metals compounds was conducted by the method of precursor carbothermic synthesis from the organic solution. ZnO:nC composites were obtained by thermolysis of succinate Zn(OO(CH2)2OO), formate glycolate Zn(HCOO)(OCH2CH2O)1/2, glycerolate Zn(OCH2CHOCH2OH), and tartrate Zn(OOCCH(OH)CH(OH)COO). WC:nC composite was synthesized from ammonium paratungstate and glycerol. In all cases, carbon structures that are specific for diamond- like carbon forms appeared on the surface of WC and ZnO particles after the heat treatment. Tungsten carbide and zinc oxide were removed from the composites by selective chemical dissolution preserving the amorphous carbon phase. This work presents the results of investigating WC:nC and ZnO:nC composites and carbon nanopowders with tubular, tape, plate and onion morphologies of aggregates that are separated by chemical dissolution of WC and ZnO from the composites by the following methods: SEM, TEM, XPA, Raman spectroscopy, and BET. The connection between the carbon morphology under the conditions of synthesis and chemical nature of the precursor and the possibility of regulation of the morphology with the specific surface area up to 1700-2000 m2/g of carbon-structured materials are discussed.

Keywords: carbon morphology, composite materials, precursor synthesis, tungsten carbide, zinc oxide

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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: Sospeter P. Maganga, Alphonce Wikedzi, Mussa D. Budeba, Samwel V. Manyele

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This study characterizes complex gold ores (elemental and mineralogical composition, gold distribution, ore grindability, and mineral liberation) for preliminary process selection. About 200 kg of ore samples were collected from each location using systematic sampling by mass interval. Ores were dried, crushed, milled, and split into representative sub-samples (about 1 kg) for elemental and mineralogical composition analyses using X-ray fluorescence (XRF), fire assay finished with Atomic Absorption Spectrometer (AAS), and X-ray Diffraction (XRD) methods, respectively. The gold distribution was studied on size-by-size fractions, while ore grindability was determined using the standard Bond test. The mineral liberation analysis was conducted using ThermoFisher Scientific Mineral Liberation Analyzer (MLA) 650, where unsieved polished grain mounts (80% passing 700 µm) were used as MLA feed. Two MLA measurement modes, X-ray modal analysis (XMOD) and sparse phase liberation-grain X-ray mapping analysis (SPL-GXMAP), were employed. At least two cyanide consumers (Cu, Fe, Pb, and Zn) and kinetics impeders (Mn, S, As, and Bi) were present in all locations investigated. Copper content at Kapanda (0.77% Cu) and Ibindi (7.48% Cu) exceeded the recommended threshold of 0.5% Cu for direct cyanidation. The gold ore at Ibindi indicated a higher rate of grinding compared to other locations. This could be explained by the highest grindability (2.119 g/rev.) and lowest Bond work index (10.213 kWh/t) values. The pyrite-marcasite, chalcopyrite, galena, and siderite were identified as major gold, copper, lead, and iron-bearing minerals, respectively, with potential for economic extraction. However, only gold and copper can be recovered under conventional milling because of grain size issues (galena is exposed by 10%) and process complexity (difficult to concentrate and smelt iron from siderite). Therefore, the preliminary process selection is copper flotation followed by gold cyanidation for Kapanda and Ibindi ores, whereas gold cyanidation with additives such as glycine or ammonia is selected for Mawemeru and Itumbi ores because of low concentrations of Cu, Pb, Fe, and Zn minerals.

Keywords: complex gold ores, mineral liberation, ore characterization, ore grindability

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Authors: Mohamed S. Selim, Nesreen A. Fatthallah, Shimaa A. Higazy, Zhifeng Hao, Ping Jing Mo

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As marine fouling-release (FR) surfaces, two new superhydrophobic nanocomposite series of polydimethylsiloxane (PDMS) loaded with reduced graphene oxide (RGO) and graphene oxide/boehmite nanorods (GO-γ-AlOOH) nanofillers were created. The self-cleaning and antifouling capabilities were modified by controlling the nanofillers' shapes and distribution in the silicone matrix. With an average diameter of 10-20 nm and a length of 200 nm, γ-AlOOH nanorods showed a single crystallinity. RGO was made using a hydrothermal process, whereas GO-γ-AlOOH nanocomposites were made using a chemical deposition method for use as fouling-release coating materials. These nanofillers were disseminated in the silicone matrix using the solution casting method to explore the synergetic effects of graphene-based materials on the surface, mechanical, and FR characteristics. Water contact angle (WCA), scanning electron, and atomic force microscopes were used to investigate the surface's hydrophobicity and antifouling capabilities (SEM and AFM). The roughness, superhydrophobicity, and surface mechanical characteristics of coatings all increased the homogeneity of the nanocomposite dispersion. To examine the antifouling effects of the coating systems, laboratory tests were conducted for 30 days using specified bacteria.PDMS/GO-γ-AlOOH nanorod composite demonstrated superior antibacterial efficacy against several bacterial strains than PDMS/RGO nanocomposite. The high surface area and stabilizing effects of the GO-γ-AlOOH hybrid nanofillers are to blame for this. The biodegradability percentage of the PDMS/GO-γ-AlOOH nanorod composite (3 wt.%) was the lowest (1.6%), while the microbial endurability percentages for gram-positive, gram-negative, and fungi were 86.42%, 97.94%, and 85.97%, respectively. The homogeneity of the GO-γ-AlOOH (3 wt.%) dispersion, which had a WCA of 151° and a rough surface, was the most profound superhydrophobic antifouling nanostructured coating.

Keywords: superhydrophobic nanocomposite, fouling release, nanofillers, surface coating

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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: B. Dejanova, S. Petrovska, L. Todorovska, J. Pluncevic, S. Mancevska, V. Antevska, E. Sivevska, I. Karagjozova

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Introduction: Aging process is mainly related to endothelial function which may be impaired by oxidative stress (OS). Exercise is known to be beneficial to aging process, which may improve health and prevent appearance of chronic diseases in elderly. The aim of the study was to investigate the OS markers related to exercise. Methods: A number of 80 subjects (healthy volunteers) were examined (38 male and 32 female), divided in 3 age groups: group I ≤ 30 years (n=24); group II – 31-50 years (n=24); group III - ≥ 51 year (n=32). Each group was divided to subgroups of sedentary subjects (SS) and subjects who exercise (SE). Group I: SS (n=11), SE (n=13); group II: SS (n=13), SE (n=10); group III: SS (n=23) SE (n=9). Lipid peroxidation (LP) as a fluorimetric method with thiobarbituric acid was used to estimate OS. Antioxidative status was determined by cell antioxidants such as enzymes - superoxide dismutase (SOD), glutathione peroxidase (GPx) and glucose 6 phosphate (G-6-PD); and by extra cell antioxidants such as glutathione reductase (GR), nitric oxide (NO) and total antioxidant capacity (TAC). Results: Increased values of LP were noticed along the aging process: group I – 3.30±0.3 µmol/L; group II – 3.91±0.2 µmol/L; group III – 3.94±0.8 µmol/L (p<0.05), while no statistical significance was found between male and female subjects. Statistical significance for OS was not found between SS and SE in group I as it was found in group II (p<0.05) and in group III (p<0.01). No statistical significance was found for all cell antioxidants and GR within the groups, while NO and TAC showed lower values in SS compared to SE in II (p<0.05) and in group III (p<0.05). Discussion and conclusion: Aging process showed increased OS which may be either due to impaired function of scavengers of free radicals or due to their enormous production. Well balanced exercise might be one of the factors that keep the integrity of blood vessel endothelium which slows down the aging process. Possible mechanism of exercise beneficial influence is shear stress by upregulation of genes coding for nitric oxide bioavailability. Thus, due to obtained results we may conclude that OS is found to be diminished in the subject groups who perform exercise.

Keywords: oxidative stress, aging process, exercise, endothelial function

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Authors: Shigenori Togashi, Yukako Asano

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We developed an effective microfluidic device for photoreactions with low reflectance and good heat conductance. The performance of this microfluidic device was tested by carrying out a photoreactive synthesis of benzopinacol and acetone from benzophenone and 2-propanol. The yield reached 36% with an irradiation time of 469.2 s and was improved by more than 30% when compared to the values obtained by the batch method. Therefore, the microfluidic device was found to be effective for improving the yields of photoreactions.

Keywords: microfluidic device, photoreaction, black aluminum oxide, benzophenone, yield improvement

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Authors: C. F. Alegretti, F. R. Cunha, R. G. Gontijo

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This work investigates the effects of an applied magnetic field on the geometry-driven boundary layer detachment flow of a ferrofluid over a sudden expansion. Both constitutive equation and global magnetization equation for a ferrofluid are considered. Therefore, the proposed formulation consists in a coupled magnetic-hydrodynamic problem. Computational simulations are carried out in order to explore, not only the viability to control flow instabilities, but also to evaluate the consistency of theoretical aspects. The unidirectional sudden expansion in a ferrofluid flow is investigated numerically under the perspective of Ferrohydrodynamics in a two-dimensional domain using a Finite Differences Method. The boundary layer detachment induced by the sudden expansion results in a recirculating zone, which has been extensively studied in non-magnetic hydrodynamic problems for a wide range of Reynolds numbers. Similar investigations can be found in literature regarding the sudden expansion under the magnetohydrodynamics framework, but none considering a colloidal suspension of magnetic particles out of the superparamagnetic regime. The vorticity-stream function formulation is implemented and results in a clear coupling between the flow vorticity and its magnetization field. Our simulations indicate a systematic decay on the length of the recirculation zone as increasing physical parameters of the flow, such as the intensity of the applied field and the volume fraction of particles. The results all are discussed from a physical point of view in terms of the dynamical non-dimensional parameters. We argue that the decrease/reduction in the recirculation region of the flow is a direct consequence of the magnetic torque balancing the action of the torque produced by viscous and inertial forces of the flow. For the limit of small Reynolds and magnetic Reynolds parameters, the diffusion of vorticity balances the diffusion of the magnetic torque on the flow. These mechanics control the growth of the recirculation region.

Keywords: boundary layer detachment, ferrofluid, ferrohydrodynamics, magnetization, sudden expansion

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Authors: Victor S. Klimin, Alexey A. Rezvan, Maxim S. Solodovnik, Oleg A. Ageev

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In this paper, the problems of existing methods of profiling and surface modification of nanoscale arsenide-gallium structures are analyzed. The use of a combination of methods of local anodic oxidation and plasma chemical etching to solve this problem is considered. The main features that make this technology one of the promising areas of modification and profiling of near-surface layers of solids are demonstrated. In this paper, we studied the effect of formation stress and etching time on the geometrical parameters of the etched layer and the roughness of the etched surface. Experimental dependences of the thickness of the etched layer on the time and stress of formation were obtained. The surface analysis was carried out using atomic force microscopy methods, the corresponding profilograms were constructed from the obtained images, and the roughness of the etched surface was studied accordingly. It was shown that at high formation voltage, the depth of the etched surface increased, this is due to an increase in the number of active particles (oxygen ions and hydroxyl groups) formed as a result of the decomposition of water molecules in an electric field, during the formation of oxide nanostructures on the surface of gallium arsenide. Oxide layers were used as negative masks for subsequent plasma chemical etching by the STE ICPe68 unit. BCl₃ was chosen as the chlorine-containing gas, which differs from analogs in some parameters for the effect of etching of nanostructures based on gallium arsenide in the low-temperature plasma. The gas mixture of reaction chamber consisted of a buffer gas NAr = 100 cm³/min and a chlorine-containing gas NBCl₃ = 15 cm³/min at a pressure P = 2 Pa. The influence of these methods modes, which are formation voltage and etching time, on the roughness and geometric parameters, and corresponding dependences are demonstrated. Probe nanotechnology was used for surface analysis.

Keywords: nanostructures, GaAs, plasma chemical etching, modification structures

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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: P. Michael Preetam Raj, Souri Banerjee, Souvik Kundu

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Oxide based memristors were fabricated in order to establish its potential applications in analog/digital electronics. BaTiO₃-BiFeO₃ (BT-BFO) was employed as an active material, whereas platinum (Pt) and Nb-doped SrTiO₃ (Nb:STO) were served as a top and bottom electrodes, respectively. Piezoelectric force microscopy (PFM) was utilized to present the ferroelectricity and repeatable polarization inversion in the BT-BFO, demonstrating its effectiveness for resistive switching. The fabricated memristors exhibited excellent electrical characteristics, such as hysteresis current-voltage (I-V), high on/off ratio, high retention time, cyclic endurance, and low operating voltages. The band-alignment between the active material BT-BFO and the substrate Nb:STO was experimentally investigated using X-Ray photoelectron spectroscopy, and it attributed to staggered heterojunction alignment. An energy band diagram was proposed in order to understand the electrical transport in BT-BFO/Nb:STO heterojunction. It was identified that the I-V curves of these memristors have several discontinuities. Curve fitting technique was utilized to analyse the I-V characteristic, and the obtained I-V equations were found to be parabolic. Utilizing this analysis, a non-linear BT-BFO memristors equivalent circuit model was developed. Interestingly, the obtained equivalent circuit of the BT-BFO memristors mimics the identical electrical performance, those obtained in the fabricated devices. Based on the developed equivalent circuit, a finite state machine (FSM) design was proposed. Efforts were devoted to fabricate the same FSM, and the results were well matched with those in the simulated FSM devices. Its multilevel noise filtering and immunity to external noise characteristics were also studied. Further, the feature of variable negative resistance was established by controlling the current through the memristor.

Keywords: band alignment, finite state machine, polarization inversion, resistive switching

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Authors: Hamidreza Khodaei, Ali Daryabeigi Zand

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Ovulation is a physiologic process with an inflammatory response that depends on a coordinated activity of gonadotropins and steroid hormones, and inflammatory mediators such as cytokines, prostaglandins, leptin, nitric oxide (NO), etc. Conjugated linoleic acid (CLA) is composed of polyunsaturated fatty acids (PUFA) found in dairy products, beef, and lamb. There is strong evidence that dietary CLA affects mediators involved in ovulation. The objective of this study is to evaluate the impacts of various doses of dietary CLA on systemic and local hormones and parameters involved in ovulation. In this case-control research, 80 (50 ± 2-day old) female mice were randomly divided into 4 groups (C as control treatment and T1, T2 and T3 are considered as the treatment groups). There were four replicates in each group, and there were five mice in every replicate (20 mice, in total). The mice in the control group were fed with no CLA in their diet, but the ones in the treatment group received 0.1, 0.3 and 0.5g/kg of CLA (replacing corn oil in the diet), respectively for four months. After that, blood samples were obtained from the tails of animals that displayed estrus signs and estradiol (E2), progesterone (P4), LH, FSH, NO, leptin and TNFα were measured. In addition, the impacts of CLA on the ovarian production of prostaglandins (PGs) and NO were studied. The data were analyzed by SAS software. CLA considerably decreased serum levels of FSH (p < 0.05), LH, estradiol, NO, leptin and TNFα (p < 0.01). In addition, CLA decreased progesterone levels, but this effect was statistically not significant. The significantly adverse effects of CLA were observed in the ovarian production of PGE2 and PGF2α (p < 0.01). It seems that CLA may play an important role in reducing the ovulation rate in mice as CLA negatively affected female reproduction and it had adverse effects on systemic and local hormones involved in ovulation.

Keywords: conjugated linoleic acid, nitric oxide, ovary, ovulation, prostaglandin, gonadotropin

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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

Procedia PDF Downloads 139

Authors: Aleksander Ejsmont, Stefan Wuttke, Joanna Goscianska

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Gaining control over particle shape, size and crystallinity is an ongoing challenge for many materials. Especially metalorganic frameworks (MOFs) are recently widely studied. Besides their remarkable porosity and interesting topologies, morphology has proven to be a significant feature. It can affect the further material application. Thus seeking new approaches that enable MOF morphology modulation is important. MOFs are reticular structures, where building blocks are made up of organic linkers and metallic nodes. The most common strategy of ensuring metal source is using salts, which usually exhibit high solubility and hinder morphology control. However, there has been a growing interest in using metal oxides as structure-directing agents towards MOFs due to their very low solubility and shape preservation. Metal oxides can be treated as a metal reservoir during MOF synthesis. Up to now, reports in which receiving MOFs from metal oxides mostly present ZnO conversion to ZIF-8. However, there are other oxides, for instance, Co₃O₄, which often is overlooked due to their structural stability and insolubility in aqueous solutions. Cobalt-based materials are famed for catalytic activity. Therefore the development of their efficient synthesis is worth attention. In the presented work, an optimized Co₃O₄transition to Co-MOFviaa solvothermal approach was proposed. The starting point of the research was the synthesis of Co₃O₄ flower petals and needles under hydrothermal conditions using different cobalt salts (e.g., cobalt(II) chloride and cobalt(II) nitrate), in the presence of urea, and hexadecyltrimethylammonium bromide (CTAB) surfactant as a capping agent. After receiving cobalt hydroxide, the calcination process was performed at various temperatures (300–500 °C). Then cobalt oxides as a source of cobalt cations were subjected to reaction with trimesic acid in solvothermal environment and temperature of 120 °C leading to Co-MOF fabrication. The solution maintained in the system was a mixture of water, dimethylformamide, and ethanol, with the addition of strong acids (HF and HNO₃). To establish how solvents affect metal oxide conversion, several different solvent ratios were also applied. The materials received were characterized with analytical techniques, including X-ray powder diffraction, energy dispersive spectroscopy,low-temperature nitrogen adsorption/desorption, scanning, and transmission electron microscopy. It was confirmed that the synthetic routes have led to the formation of Co₃O₄ and Co-based MOF varied in shape and size of particles. The diffractograms showed receiving crystalline phase for Co₃O₄, and also for Co-MOF. The Co₃O₄ obtained from nitrates and with using low-temperature calcination resulted in smaller particles. The study indicated that cobalt oxide particles of different size influence the efficiency of conversion and morphology of Co-MOF. The highest conversion was achieved using metal oxides with small crystallites.

Keywords: Co-MOF, solvothermal synthesis, morphology control, core-shell

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Authors: Abbas Kamalibandpey, Alain Beland, Joseph Mukendi Kabuya

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Since a rock mass is a discontinuum medium, its behaviour is governed by discontinuities such as faults, joint sets, lithologic contact, and bedding planes. Thus, rock slope stability analysis in jointed rock masses is largely dependent upon discontinuities constitutive equations. This paper studies the difference between the Mohr-Coulomb (MC) and the Barton-Bandis (BB) joint constitutive numerical models for lithological contacts and joint sets. For the rock in these models, generalized Hoek-Brown criteria have been considered. The joint roughness coefficient (JRC) and the joint wall compressive strength (JCS) are vital parameters in the BB model. The numerical models are applied to the rock slope stability analysis in the Mont-Wright (MW) mine. The Mont-Wright mine is owned and operated by ArcelorMittal Mining Canada (AMMC), one of the largest iron-ore open pit operations in Canada. In this regard, one of the high walls of the mine has been selected to undergo slope stability analysis with RS2D software, finite element method. Three piezometers have been installed in this zone to record pore water pressure and it is monitored by radar. In this zone, the AMP-IF and QRMS-IF contacts and very persistent and altered joint sets in IF control the rock slope behaviour. The height of the slope is more than 250 m and consists of different lithologies such as AMP, IF, GN, QRMS, and QR. To apply the B-B model, the joint sets and geological contacts have been scanned by Maptek, and their JRC has been calculated by different methods. The numerical studies reveal that the JRC of geological contacts, AMP-IF and QRMS-IF, and joint sets in IF had a significant influence on the safety factor. After evaluating the results of rock slope stability analysis and the radar data, the B-B constitutive equation for discontinuities has shown acceptable results to the real condition in the mine. It should be noted that the difference in safety factors in MC and BB joint constitutive models in some cases is more than 30%.

Keywords: barton-Bandis criterion, Hoek-brown and Mohr-Coulomb criteria, open pit, slope stability

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Authors: Reza Vakili, Xiaolei Fan, Alex Walton

Abstract:

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: Sahin Yakut, H. Kemal Ulutas, Deniz Deger

Abstract:

Plasma Assisted Physical Vapor Deposition (PAPVD) method used to produce Poly(ethylene oxide) (pPEO) thin films. Depositions were progressed at various plasma discharge powers as 0, 2, 5 and 30 W for pPEO at 500nm film thicknesses. The capacitance and dielectric dissipation of the thin films were measured at 0,1-107 Hz frequency range and 173-353 K temperature range by an impedance analyzer. Then, alternative conductivity (σac) and activation energies were derived from capacitance and dielectric dissipation. σac of conventional PEO (PEO precursor) was measured to determine the effect of plasma discharge. Differences were observed between the alternative conductivity of PEO’s and pPEO’s depending on plasma discharge power. By this purpose, structural characterization techniques such as Differential Scanning Calorimetry (DSC) and Fourier Transform Infrared Spectroscopy (FT-IR) were applied on pPEO thin films. Structural analysis showed that density of crosslinking is plasma power dependent. The crosslinking density increases with increasing plasma discharge power and this increase is displayed as increasing dynamic glass transition temperatures at DSC results. Also, shifting of frequencies of some type of bond vibrations, belonging to bond vibrations produced after fragmentation because of plasma discharge, were observed at FTIR results. The dynamic glass transition temperatures obtained from alternative conductivity results for pPEO consistent with the results of DSC. Activation energies exhibit Arrhenius behavior. Activation energies decrease with increasing plasma discharge power. This behavior supports the suggestion expressing that long polymer chains and long oligomers are fragmented into smaller oligomers or radicals.

Keywords: activation energy, dielectric spectroscopy, organic thin films, plasma polymer

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