Search results for: nickel oxides

Authors: Ravindra P. Singh, Drupad Ram, Dinesh K. Gupta

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Rare earth ions doped metal oxides are a class of luminescent materials which have been proved to be excellent for applications in field emission displays and cathode ray tubes, plasma display panels. Under UV irradiation Eu+++ doped Y2O3 is a red phosphor and Tb+++ doped Y 2O3 is a green phosphor. It is possible that, due to their high quantum efficiency, they might serve as improved luminescent markers for identification of biomolecules, as already reported for CdSe and CdSe/ZnS nanocrystals. However, for any biological applications these particle powders must be suspended in water while retaining their phosphorescence. We hereby report synthesis and characterization of Eu+++ and Tb+++ doped yttrium oxide nanoparticles by sol-gel and hydrothermal processes. Eu+++ and Tb+++ doped Y2O3 nanoparticles have been synthesized by hydrothermal process using yttrium oxo isopropoxide [Y5O(OPri)13] (crystallized twice) and it’s acetyl acetone modified product [Y(O)(acac)] as precursors. Generally the sol-gel derived metal oxides are required to be annealed to the temperature ranging from 400°C-800°C in order to develop crystalline phases. However, this annealing also results in the development of aggregates which are undesirable for bio-conjugation experiments. In the hydrothermal process, we have achieved crystallinity of the nanoparticles at 300°C and the development of crystalline phases has been found to be proportional to the time of heating of the reactor. The average particle sizes as calculated from XRD were found to be 28 nm, 32 nm, and 34 nm by hydrothermal process. The particles were successfully suspended in chloroform in the presence of trioctyl phosphene oxide and TEM investigations showed the presence of single particles along with agglomerates.

Keywords: nanophosphors, Y2O3:Eu+3, Y2O3:Tb+3, sol-gel, hydrothermal method, TEM, XRD

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Authors: Kirill M. Dubovikov, Ekaterina S. Marchenko, Gulsharat A. Baigonakova

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NiTi alloys are widely used as implants in medicine due to their unique properties such as superelasticity, shape memory effect and biocompatibility. However, despite these properties, one of the major problems is the release of nickel after prolonged use in the human body under dynamic stress. This occurs due to oxidation and cracking of NiTi implants, which provokes nickel segregation from the matrix to the surface and release into living tissues. As we know, nickel is a toxic element and can cause cancer, allergies, etc. One of the most popular ways to solve this problem is to create a corrosion resistant coating on NiTi. There are many coatings of this type, but not all of them have good biocompatibility, which is very important for medical implants. Coatings based on calcium phosphate phases have excellent biocompatibility because Ca and P are the main constituents of the mineral part of human bone. This fact suggests that a Ca-P coating on NiTi can enhance osteogenesis and accelerate the healing process. Therefore, the aim of this study is to investigate the structure of Ca-P coating on NiTi substrate. Plasma assisted radio frequency (RF) sputtering was used to obtain this film. This method was chosen because it allows the crystallinity and morphology of the Ca-P coating to be controlled by the sputtering parameters. It allows us to obtain three different NiTi samples with Ca-P coating. XRD, AFM, SEM and EDS were used to study the composition, structure and morphology of the coating phase. Scratch tests were carried out to evaluate the adhesion of the coating to the substrate. Wettability tests were used to investigate the hydrophilicity of the different coatings and to suggest which of them had better biocompatibility. XRD showed that the coatings of all samples were hydroxyapatite, but the matrix was represented by TiNi intermetallic compounds such as B2, Ti2Ni and Ni3Ti. The SEM shows that the densest and defect-free coating has only one sample after three hours of sputtering. Wettability tests show that the sample with the densest coating has the lowest contact angle of 40.2° and the largest free surface area of 57.17 mJ/m2, which is mostly disperse. A scratch test was carried out to investigate the adhesion of the coating to the surface and it was shown that all coatings were removed by a cohesive mechanism. However, at a load of 30N, the indenter reached the substrate in two out of three samples, except for the sample with the densest coating. It was concluded that the most promising sputtering mode was the third, which consisted of three hours of deposition. This mode produced a defect-free Ca-P coating with good wettability and adhesion.

Keywords: biocompatibility, calcium phosphate coating, NiTi alloy, radio frequency sputtering.

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Authors: Chun-Ying Lee, Kun-Hsien Lee, Bor-Wei Wang

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The process of post-supercritical CO₂ electroplating uses the electrolyte solution after being mixed with supercritical CO₂ and released to atmospheric pressure. It utilizes the microbubbles that form when oversaturated CO₂ in the electrolyte returns to gaseous state, which gives the similar effect of pulsed electroplating. Under atmospheric pressure, the CO₂ bubbles gradually diffuse. Therefore, the introduction of ultrasound and/or other agitation can potentially excite the CO₂ microbubbles to achieve an electroplated surface of even higher quality. In this study, during the electroplating process, three different modes of agitation: magnetic stirrer agitation, ultrasonic agitation and a combined mode (magnetic + ultrasonic) were applied, respectively, in order to obtain an optimal surface morphology and mechanical properties for the electroplated Ni coating. It is found that the combined agitation mode at a current density of 40 A/dm² achieved the smallest grain size, lower surface roughness, and produced an electroplated Ni layer that achieved hardness of 320 HV, much higher when compared with conventional method, which were usually in the range of 160 to 300 HV. However, at the same time, the electroplating with combined agitation developed a higher internal stress of 320 MPa due to the lower current efficiency of the process and finer grain in the coating. Moreover, a new control methodology for tailoring the coating’s mechanical property through its thickness was demonstrated by the timely introduction of ultrasonic agitation during the electroplating process with post supercritical CO₂ mixed electrolyte.

Keywords: nickel electroplating, micro-bubbles, supercritical carbon dioxide, ultrasonic agitation

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Authors: O. Adjroud

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The present study was conducted to investigate the interaction between selenium (Se) and chloride nickel (NiCl2) on energy profiles in Wistar albino preimplanted rats. NiCl2 was given on day 3 of pregnancy either in distilled drinking water at a dose of 20 mg/L/day for 16 consecutive days or as a single subcutaneous (s.c.) dose of 25, 50, or 100 mg/kg. Se was given as a s.c. injection (0.3 mg/kg) together with the higher dose (100 mg/kg) of NiCl2. Changes in energy profiles were evaluated in treated and control groups on days 5 and 20 of gestation. NiCl2 s.c. induced a significant increase in plasma glucose on day 20 of pregnancy. NiCl2 s.c. induced on day 5 and 20 of gestation a significant decrease in plasma triglycerides, with the higher dose. This decrease was maintained at day 20 of gestation with doses of 50 mg /kg. In addition, NiCl2 s.c. caused on day 5 of gestation a significant decrease in plasma total cholesterol with the low and medium doses. The pretreatment with Se reversed the effects of NiCl2 on plasma glucose, total cholesterol and triglycerides levels. NiCl2 administered in the drinking water augmented significantly the plasma triglycerides and total cholesterol levels and slighty the plasma glucose on day 20 of gestation, while on day 5 of gestation NiCl2 s.c. Induced a significant decrease in cholesterol. Three doses of NiCl2 (sc) induced severe alterations in liver and architecture which are markedly improved by Selenium. These results suggested that selenium has protective effects on energy profiles against the toxicity induced by NiCl2 administered subcutaneously in preimplanted rats.

Keywords: hepatotoxicity, nickel chloride, preimplanted rat, biochemical parameters

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Authors: Z. Jamalzadeh, A. Niaei, H. Erfannia, S. G. Hosseini, A. S. Razmgir

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Due to developing the industries, the emission of pollutants such as NOx, SOx, and CO2 are rapidly increased. Generally, NOx is attributed to the mono nitrogen oxides of NO and NO2 that is one of the most important atmospheric contaminants. Hence, controlling the emission of nitrogen oxides is urgent environmentally. Selective Catalytic Reduction of NOx is one of the most common techniques for NOx removal in which Zeolites have wide application due to their high performance. In zeolitic processes, the catalytic reaction occurs mostly in the pores. Therefore, investigation the adsorption phenomena of the molecules in order to gain an insight and understand the catalytic cycle is of important. Hence, in current study, molecular simulations is applied for studying the adsorption phenomena in nanocatalysts applied for SCR of NOx process. The effect of cation addition to the support in the catalysts’ behavior through adsorption step was explored by Mont Carlo (MC). Simulation time of 1 Ns accompanying 1 fs time step, COMPASS27 Force Field and the cut off radios of 12.5 Ȧ was applied for performed runs. It was observed that the adsorption capacity increases in the presence of cations. The sorption isotherms demonstrated the behavior of type I isotherm categories and sorption capacity diminished with increase in temperature whereas an increase was observed at high pressures. Besides, NO sorption showed higher sorption capacity than NH3 in H–ZSM5. In this respect, the Energy distributions signified that the molecules could adsorb in just one sorption site at the catalyst and the sorption energy of NO was stronger than the NH3 in H-ZSM5. Furthermore, the isosteric heat of sorption data showed nearly same values for the molecules; however, it indicated stronger interactions of NO molecules with H-ZSM5 Zeolite compared to the isosteric heat of NH3 which was low in value.

Keywords: Monte Carlo simulation, adsorption, NOx, ZSM5

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Authors: Hyeonseok Yoo, Kiseok Oh, Jinsub Choi

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Titanium oxide nanotubes have attracted great attention because of its photocatalytic activity and large surface area. For enhancing electrochemical properties, catalysts should be doped into the structure because titanium oxide nanotubes themselves have low electroconductivity and catalytic activity. It has been reported that Ru and Ir doped titanium oxide electrodes exhibit high efficiency and low overpotential in the oxygen evolution reaction (OER) for water splitting. In general, titanium oxide nanotubes with high aspect ratio cannot be easily doped by conventional complex methods. Herein, two types of facile routes, namely single step anodization and potential shock, for Ru doping into high aspect ratio titanium oxide nanotubes are introduced in detail. When single step anodization was carried out, stability of electrodes were increased. However, onset potential was shifted to anodic direction. On the other hand, when high potential shock voltage was applied, a large amount of ruthenium/ruthenium oxides were doped into titanium oxide nanotubes and thick barrier oxide layers were formed simultaneously. Regardless of doping routes, ruthenium/ ruthenium oxides were homogeneously doped into titanium oxide nanotubes. In spite of doping routes, doping in aqueous solution generally led to incorporate high amount of Ru in titanium oxide nanotubes, compared to that in non-aqueous solution. The amounts of doped catalyst were analyzed by X-ray photoelectron spectroscopy (XPS). The optimum condition for water splitting was investigated in terms of the amount of doped Ru and thickness of barrier oxide layer.

Keywords: doping, potential shock, single step anodization, titanium oxide nanotubes

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Authors: G. Singh, H.Schuster, U. Füssel

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The stability of electric arc and durability of electrode tip used in Tungsten Inert Gas (TIG) welding demand a metallurgical study about the chemical transport mechanism of emitter oxide particles in tungsten electrode during its real welding conditions. The tungsten electrodes doped with emitter oxides of rare earth oxides such as La₂O₃, Th₂O₃, Y₂O₃, CeO₂ and ZrO₂ feature a comparatively lower work function than tungsten and thus have superior emission characteristics due to lesser surface temperature of the cathode. The local change in concentration of these emitter particles in tungsten electrode due to high temperature diffusion (chemical transport) can change its functional properties like electrode temperature, work function, electron emission, and stability of the electrode tip shape. The resulting increment in tip surface temperature results in the electrode material loss. It was also observed that the tungsten recrystallizes to large grains at high temperature. When the shape of grain boundaries are granular in shape, the intergranular diffusion of oxide emitter particles takes more time to reach the electrode surface. In the experimental work, the microstructure of the used electrode's tip surface will be studied by scanning electron microscope and reflective X-ray technique in order to gauge the extent of the diffusion and chemical reaction of emitter particles. Besides, a simulated model is proposed to explain the effect of oxide particles diffusion on the electrode’s microstructure, electron emission characteristics, and electrode tip erosion. This model suggests metallurgical modifications in tungsten electrode to enhance its erosion resistance.

Keywords: rare-earth emitter particles, temperature-dependent diffusion, TIG welding, Tungsten electrode

Procedia PDF Downloads 158

Authors: Z. Jamalzadeh, A. Niaei, H. Erfannia

Abstract:

Due to developing industries, the emission of pollutants such as NOx, SOx, and CO2 are rapidly increased. Generally, NOx is attributed to the mono nitrogen oxides of NO and NO2 that is one of the most important atmospheric contaminants. Hence, controlling the emission of nitrogen oxides is environmentally urgent. Selective catalytic reduction of NOx is one of the most common techniques for NOx removal in which zeolites have wide application due to their high performance. In zeolitic processes, the catalytic reaction occurs mostly in the pores. Therefore, investigation of the adsorption phenomena of the molecules in order to gain an insight and understand the catalytic cycle is of important. Hence, in current study, benefiting from molecular simulations, the adsorption phenomena in the nanocatalysts of SCR of NOx process was investigated in order to get a good insight of the catalysts’ behavior. The effect of cation addition to the support in the catalysts’ behavior through adsorption step was explored by Mont Carlo (MC) using Materials Studio Package. Simulation time of 1 Ns accompanying 1 fs time step, COMPASS27 Force Field and the cut off radios of 12.5 Ȧ was applied for performed runs. It was observed that the adsorption capacity increases in the presence of cations. The sorption isotherms demonstrated the behavior of type I isotherm categories and sorption capacity diminished with increase in temperature whereas an increase was observed at high pressures. Besides, NO sorption showed higher sorption capacity than NH3 in H–ZSM5. In this respect, the energy distributions signified that the molecules could adsorb in just one sorption site at the catalyst and the sorption energy of NO was stronger than the NH3 in H-ZSM5. Furthermore, the isosteric heat of sorption data showed nearly same values for the molecules; however, it indicated stronger interactions of NO molecules with H-ZSM5 zeolite compared to the isosteric heat of NH3 which was low in value.

Keywords: Monte Carlo simulation, adsorption, NOx, ZSM5

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Authors: Chinwendu R. Nnabalu, Gioia Falcone, Imma Bortone

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Petroleum refining is a chemical process in which the raw material (crude oil) is converted to finished commercial products for end users. The fluid catalytic cracking (FCC) unit is a key asset in refineries, requiring optimised processes in the context of engineering design. Following the first stage of separation of crude oil in a distillation tower, an additional 40 per cent quantity is attainable in the gasoline pool with further conversion of the downgraded product of crude oil (residue from the distillation tower) using a catalyst in the FCC process. Effective removal of sulphur oxides, nitrogen oxides, carbon and heavy metals from FCC gasoline requires greater separation efficiency and involves an enormous environmental significance. The FCC unit is primarily a reactor and regeneration system which employs cyclone systems for separation.  Catalyst losses in FCC cyclones lead to high particulate matter emission on the regenerator side and fines carryover into the product on the reactor side. This paper aims at demonstrating the importance of FCC unit design criteria in terms of technical performance and compliance with environmental legislation. A systematic review of state-of-the-art FCC technology was carried out, identifying its key technical challenges and sources of emissions.  Case studies of petroleum refineries in Nigeria were assessed against selected global case studies. The review highlights the need for further modelling investigations to help improve FCC design to more effectively meet product specification requirements while complying with stricter environmental legislation.

Keywords: design, emission, fluid catalytic cracking, petroleum refineries

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Authors: P. Acosta-Santamaría, A. Ibatá-Soto, A. López-Vásquez

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Organic compounds in wastewaters coming from textile and pharmaceutical industry generated multiple harmful effects on the environment and the human health. One of them is the methyl orange (MeO), an azoic dye considered to be a recalcitrant compound. The heterogeneous photocatalysis emerges as an alternative for treating this type of hazardous compounds, through the generation of OH radicals using radiation and a semiconductor oxide. According to the author’s knowledge, catalysts such as TiO₂ doped with metals show high efficiency in degrading MeO; however, this presents economic limitations on industrial scale. Black sand can be considered as a naturally doped catalyst because in its structure is common to find compounds such as titanium, iron and aluminum oxides, also elements such as zircon, cadmium, manganese, etc. This study reports the photocatalytic activity of the mineral black sand used as semiconductor in the discoloration of MeO by oxidation and reduction photocatalytic techniques. For this, magnetic composites from the mineral were prepared (RM, M1, M2 and NM) and their activity were tested through MeO discoloration while TiO₂ was used as reference. For the fractions, chemical, morphological and structural characterizations were performed using Scanning Electron Microscopy with Energy Dispersive X-Ray (SEM-EDX), X-Ray Diffraction (XRD) and X-Ray Fluorescence (XRF) analysis. M2 fraction showed higher MeO discoloration (93%) in oxidation conditions at pH 2 and it could be due to the presence of ferric oxides. However, the best result to reduction process was using M1 fraction (20%) at pH 2, which contains a higher titanium percentage. In the first process, hydrogen peroxide (H₂O₂) was used as electron donor agent. According to the results, black sand mineral can be used as natural semiconductor in photocatalytic process. It could be considered as a photocatalyst precursor in such processes, due to its low cost and easy access.

Keywords: black sand mineral, methyl orange, oxidation, photocatalysis, reduction

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Authors: Abdoulaye Maihatchi Ahamed, Zubin Arora, Benjamin Swobada, Jean-yves Lansot, Alexandre Chagnes

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Lithium-ion battery (LiB) is the technology of choice in the development of electric vehicles. But there are still many challenges, including the development of positive electrode materials exhibiting high cycle ability, high energy density, and low environmental impact. For this latter, LiBs must be manufactured in a circular approach by developing the appropriate strategies to reuse and recycle them. Presently, the recycling of LiBs is carried out by the pyrometallurgical route, but more and more processes implement or will implement the hydrometallurgical route or a combination of pyrometallurgical and hydrometallurgical operations. After producing the black mass by mineral processing, the hydrometallurgical process consists in leaching the black mass in order to uptake the metals contained in the cathodic material. Then, these metals are extracted selectively by liquid-liquid extraction, solid-liquid extraction, and/or precipitation stages. However, liquid-liquid extraction combined with precipitation/crystallization steps is the most implemented operation in the LiB recycling process to selectively extract copper, aluminum, cobalt, nickel, manganese, and lithium from the leaching solution and precipitate these metals as high-grade sulfate or carbonate salts. Liquid-liquid extraction consists in contacting an organic solvent and an aqueous feed solution containing several metals, including the targeted metal(s) to extract. The organic phase is non-miscible with the aqueous phase. It is composed of an extractant to extract the target metals and a diluent, which is usually aliphatic kerosene produced from the petroleum industry. Sometimes, a phase modifier is added in the formulation of the extraction solvent to avoid the third phase formation. The extraction properties of the diluent do not depend only on the chemical structure of the extractant, but it may also depend on the nature of the diluent. Indeed, the interactions between the diluent can influence more or less the interactions between extractant molecules besides the extractant-diluent interactions. Only a few studies in the literature addressed the influence of the diluent on the extraction properties, while many studies focused on the effect of the extractants. Recently, new low-carbon footprint aliphatic diluents were produced by catalytic dearomatisation and distillation of bio-based oil. This study aims at investigating the influence of the nature of the diluent on the extraction properties of three extractants towards cobalt, nickel, manganese, copper, aluminum, and lithium: Cyanex®272 for nickel-cobalt separation, DEHPA for manganese extraction, and Acorga M5640 for copper extraction. The diluents used in the formulation of the extraction solvents are (i) low-odor aliphatic kerosene produced from the petroleum industry (ELIXORE 180, ELIXORE 230, ELIXORE 205, and ISANE IP 175) and (ii) bio-sourced aliphatic diluents (DEV 2138, DEV 2139, DEV 1763, DEV 2160, DEV 2161 and DEV 2063). After discussing the effect of the diluents on the extraction properties, this conference will address the development of a low carbon footprint process based on the use of the best bio-sourced diluent for the production of high-grade cobalt sulfate, nickel sulfate, manganese sulfate, and lithium carbonate, as well as metal copper.

Keywords: diluent, hydrometallurgy, lithium-ion battery, recycling

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Authors: Bekan Bogale, Tsegaye Girma Asere, Tilahun Yai, Fekadu Melak

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Aims: To study photocatalytic degradation of methylene blue dye on cuprous oxide/graphene nanocomposite. Background: Cuprous oxide (Cu2O) nanoparticles are among the metal oxides that demonstrated photocatalytic activity. However, the stability of Cu2O nanoparticles due to the fast recombination rate of electron/hole pairs remains a significant challenge in their photocatalytic applications. This, in turn, leads to mismatching of the effective bandgap separation, tending to reduce the photocatalytic activity of the desired organic waste (MB). To overcome these limitations, graphene has been combined with cuprous oxides, resulting in cuprous oxide/graphene nanocomposite as a promising photocatalyst. Objective: In this study, Cu2O/graphene nanocomposite was synthesized and evaluated for its photocatalytic performance of methylene blue (MB) dye degradation. Method: Cu2O/graphene nanocomposites were synthesized from graphite powder and copper nitrate using the facile sol-gel method. Batch experiments have been conducted to assess the applications of the nanocomposites for MB degradation. Parameters such as contact time, catalyst dosage, and pH of the solution were optimized for maximum MB degradation. The prepared nanocomposites were characterized by using UV-Vis, FTIR, XRD, and SEM. The photocatalytic performance of Cu2O/graphene nanocomposites was compared against Cu2O nanoparticles for cationic MB dye degradation. Results: Cu2O/graphene nanocomposite exhibits higher photocatalytic activity for MB degradation (with a degradation efficiency of 94%) than pure Cu2O nanoparticles (67%). This has been accomplished after 180 min of irradiation under visible light. The kinetics of MB degradation by Cu2O/graphene composites can be demonstrated by the second-order kinetic model. The synthesized nanocomposite can be used for more than three cycles of photocatalytic MB degradation. Conclusion: This work indicated new insights into Cu2O/graphene nanocomposite as high-performance in photocatalysis to degrade MB, playing a great role in environmental protection in relation to MB dye.

Keywords: methylene blue, photocatalysis, cuprous oxide, graphene nanocomposite

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Authors: Anna-Caroline Lavergne-Bril, Jean-François Colin, David Peralta, Pascale Maldivi

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Cobalt is a critical material, widely used in Li-ion batteries. Due to the planned electrification of European vehicles, cobalt needs are expending – and resources are limited. To meet the needs in cobalt to come, it is necessary to develop new efficient ways to recycle cobalt. One of the biggest sources comes from old electrical vehicles batteries (batteries sold in 2019: 500 000 tons of waste to be). A closed loop process of cobalt recycling has been developed and this presentation aims to present the selectivity mechanism of cobalt over manganese and nickel in solution. Cobalt precipitation as a ZIF material (Zeolitic Imidazolate framework) from a starting solution composed of equimolar nickel, manganese and cobalt is studied. A 2-MeIm (2-methylimidazole) linker is introduced in a multimetallic Ni, Mn, Co solution and the resulting ZIF-67 is 100% pure Co among its metallic centers. Selectivity of Co over Ni is experimentally studied and DFT modelisation calculation are conducted to understand the geometry of ligand-metal-solvent complexes in solution. Selectivity of Co over Mn is experimentally studied, and DFT modelisation calcucation are conducted to understand the link between pKa of the ligand and precipitration of Mn impurities within the final material. Those calculation open the way to other ligand being used in the same process, with more efficiency. Experimental material are synthetized from bimetallic (Ni²⁺/Co²⁺, Mn²⁺/Co²⁺, Mn²⁺/Ni²⁺) solutions. Their crystallographic structure is analysed by XRD diffraction (Brüker AXS D8 diffractometer, Cu anticathode). Morphology is studied by scanning electron microscopy, using a LEO 1530 FE-SEM microscope. The chemical analysis is performed by using ICP-OES (Agilent Technologies 700 series ICP-OES). Modelisation calculation are DFT calculation (density functional theory), using B3LYP, conducted with Orca 4.2.

Keywords: MOFs, ZIFs, recycling, closed-loop, cobalt, li-ion batteries

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Authors: M. Zielinska, B. Daniels, J. Gabel, A. Paletko

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A common nickel based superalloy Inconel625 was brazed with Ni-base braze filler material (AMS4777) containing melting-point-depressants such as B and Si. Different braze gaps, brazing times and forms of braze filler material were tested. It was determined that the melting point depressants B and Si tend to form hard and brittle phases in the joint during the braze cycle. Brittle phases significantly reduce mechanical properties (e. g. tensile strength) of the joint. Therefore, it is important to define optimal process parameters to achieve high strength joints, free of brittle phases. High ultimate tensile strength (UTS) values can be obtained if the joint area is free of brittle phases, which is equivalent to a complete isothermal solidification of the joint. Isothermal solidification takes place only if the concentration of the melting point depressant in the braze filler material of the joint is continuously reduced by diffusion into the base material. For a given brazing temperature, long brazing times and small braze filler material volumes (small braze gaps) are beneficial for isothermal solidification. On the base of the obtained results it can be stated that the form of the braze filler material has an additional influence on the joint quality. Better properties can be achieved by the use of braze-filler-material in form of foil instead of braze-filler-material in form of paste due to a reduced amount of voids and a more homogeneous braze-filler-material-composition in the braze-gap by using foil.

Keywords: diffusion brazing, microstructure, superalloy, tensile strength

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Authors: Roussin Lontio Fomekong, John Lambi Ngolui, Arnaud Dercorte

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Current years have seen increased interest in the synthesis of p/n metal oxide-based nano composites and their great potential in advanced applications, such as opto electronics, photo catalysis and gas sensors. The superior functional performances of the system combining p-type and n-types semiconducting oxyde in comparison to the corresponding single-phase metal oxides are mainly ascribed to the build-up of an inner electric field at the p/n junction interface.

Keywords: nanocomposite, semiconductors, p-n, heterojunction

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Authors: Ece A. Irmak, Amdulla O. Mekhrabov, M. Vedat Akdeniz

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There is a growing interest on the synthesis and characterization of nanoalloys since the unique chemical, and physical properties of nanoalloys can be tuned and, consequently, new structural motifs can be created by varying the type of constituent elements, atomic and magnetic ordering, as well as size and shape of the nanoparticles. Due to the fine size effects, magnetic nanoalloys have considerable attention with their enhanced mechanical, electrical, optical and magnetic behavior. As an important magnetic nanoalloy, the novel application area of Fe-Ni based nanoalloys is expected to be widened in the chemical, aerospace industry and magnetic biomedical applications. Noble metals have been using in biomedical applications for several years because of their surface plasmon properties. In this respect, iron-nickel nanoalloys are promising materials for magnetic biomedical applications because they show novel properties such as superparamagnetism and surface plasmon resonance property. Also, there is great attention for the usage Fe-Ni based nanoalloys as radar absorbing materials in aerospace and stealth industry due to having high Curie temperature, high permeability and high saturation magnetization with good thermal stability. In this study, FeNi₃ bimetallic nanoalloys were synthesized by mechanical alloying in a planetary high energy ball mill. In mechanical alloying, micron size powders are placed into the mill with milling media. The powders are repeatedly deformed, fractured and alloyed by high energy collision under the impact of balls until the desired composition and particle size is achieved. The experimental studies were carried out in two parts. Firstly, dry mechanical alloying with high energy dry planetary ball milling was applied to obtain FeNi₃ nanoparticles. Secondly, dry milling was followed by surfactant-assisted ball milling to observe the surfactant and solvent effect on the structure, size, and properties of the FeNi₃ nanoalloys. In the first part, the powder sample of iron-nickel was prepared according to the 1:3 iron to nickel ratio to produce FeNi₃ nanoparticles and the 1:10 powder to ball weight ratio. To avoid oxidation during milling, the vials had been filled with Ar inert gas before milling started. The powders were milled for 80 hours in total and the synthesis of the FeNi₃ intermetallic nanoparticles was succeeded by mechanical alloying in 40 hours. Also, regarding the particle size, it was found that the amount of nano-sized particles raised with increasing milling time. In the second part of the study, dry milling of the Fe and Ni powders with the same stoichiometric ratio was repeated. Then, to prevent agglomeration and to obtain smaller sized nanoparticles with superparamagnetic behavior, surfactants and solvent are added to the system, after 40-hour milling time, with the completion of the mechanical alloying. During surfactant-assisted ball milling, heptane was used as milling medium, and as surfactants, oleic acid and oleylamine were used in the high energy ball milling processes. The characterization of the alloyed particles in terms of microstructure, morphology, particle size, thermal and magnetic properties with respect to milling time was done by X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy, vibrating-sample magnetometer, and differential scanning calorimetry.

Keywords: iron-nickel systems, magnetic nanoalloys, mechanical alloying, nanoalloy characterization, surfactant-assisted ball milling

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Authors: Valentina Paolucci, Jessica De Santis, Vittorio Ricci, Giacomo Giorgi, Carlo Cantalini

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Despite their potential in gas sensing applications, the major drawback of 2D exfoliated metal dichalcogenides (MDs) is that they suffer from spontaneous oxidation in air, showing poor chemical stability under dry/wet conditions even at room temperature, limiting their practical exploitation. The aim of this work is to validate a synthesis strategy allowing microstructural and electrical stabilization of the oxides that inevitably form on the surface of 2D dichalcogenides. Taking advantage of spontaneous oxidation of MDs in air, we report on liquid phase exfoliated 2D-SnSe2 flakes annealed in static air at a temperature below the crystallization temperature of the native a-SnO2 oxide. This process yields a new class of 2D Layered Amorphous Metal Oxides Sensors (LAMOS), specifically few-layered amorphous a-SnO2, showing excellent gas sensing properties. Sensing tests were carried out at low operating temperature (i.e. 100°C) by exposing a-SnO2 to both oxidizing and reducing gases (i.e. NO2, H2S and H2) and different relative humidities ranging from 40% to 80% RH. The formation of stable nanosheets of amorphous a-SnO2 guarantees excellent reproducibility and stability of the response over one year. These results pave the way to new interesting research perspectives out considering the opportunity to synthesize homogeneous amorphous textures with no grain boundaries, no grains, no crystalline planes with different orientations, etc., following gas sensing mechanisms that likely differ from that of traditional crystalline metal oxide sensors. Moreover, the controlled annealing process could likely be extended to a large variety of Transition Metal Dichalcogenides (TMDs) and Metal Chalcogenides (MCs), where sulfur, selenium, or tellurium atoms can be easily displaced by O2 atoms (ΔG < 0), enabling the synthesis of a new family of amorphous interfaces.

Keywords: layered 2D materials, exfoliation, lamos, amorphous metal oxide sensors

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Authors: F. Z. Tighilt, N. Belhaneche-Bensemra, S. Belhousse, S. Sam, K. Lasmi, N. Gabouze

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Recently, the gold nanoparticles (Au NPs) became an active multidisciplinary research topic. First, Au thin films fabricated by alkylthiol-functionalized Au NPs were found to have vapor sensitive conductivities, they were hence widely investigated as electrical chemiresistors for sensing different vapor analytes and even organic molecules in aqueous solutions. Second, Au thin films were demonstrated to have speciallocalized surface plasmon resonances (LSPR), so that highly ordered 2D Au superlattices showed strong collective LSPR bands due to the near-field coupling of adjacent nanoparticles and were employed to detect biomolecular binding. Particularly when alkylthiol ligands were replaced by thiol-terminated polymers, the resulting polymer-modified Au NPs could be readily assembled into 2D nanostructures on solid substrates. Monolayers of polystyrene-coated Au NPs showed typical dipolar near-field interparticle plasmon coupling of LSPR. Such polymer-modified Au nanoparticle films have an advantage that the polymer thickness can be feasibly controlled by changing the polymer molecular weight. In this article, the effect of tin-doped indium oxide (ITO) coatings on the plasmonic properties of ITO interfaces modified with gold nanostructures (Au NSs) is investigated. The interest in developing ITO overlayers is multiple. The presence of a con-ducting ITO overlayer creates a LSPR-active interface, which can serve simultaneously as a working electrode in an electro-chemical setup. The surface of ITO/ Au NPs contains hydroxyl groups that can be used to link functional groups to the interface. Here the covalent linking of nickel /Au NSs/ITO hybrid LSPR platforms will be presented.

Keywords: conducting polymer, metal nanoparticles (NPs), LSPR, poly (3-(pyrrolyl)–carboxylic acid), polypyrrole

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Authors: A. E. Mukhametov, M. T. Yerbulekova, D. R. Dautkanova, G. A. Tuyakova, G. Aitkhozhayeva

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The accumulation of heavy metals in food is a constant problem in many parts of the world. Vegetable oils are widely used, both for cooking and for processing in the food industry, meeting the main dietary requirements. One of the main chemical pollutants, heavy metals, is usually found in vegetable oils. These chemical pollutants are carcinogenic, teratogenic and immunotoxic, harmful to consumption and have a negative effect on human health even in trace amounts. Residues of these substances can easily accumulate in vegetable oil during cultivation, processing and storage. In this article, the content of the concentration of heavy metal ions in vegetable oils of Kazakhstan production is studied: sunflower, rapeseed, safflower and linseed oil. Heavy metals: arsenic, cadmium, lead and nickel, were determined in three repetitions by the method of flame atomic absorption. Analysis of vegetable oil samples revealed that the largest lead contamination (Pb) was determined to be 0.065 mg/kg in linseed oil. The content of cadmium (Cd) in the largest amount of 0.009 mg/kg was found in safflower oil. Arsenic (As) content was determined in rapeseed and safflower oils at 0.003 mg/kg, and arsenic (As) was not detected in linseed and sunflower oil. The nickel (Ni) content in the largest amount of 0.433 mg/kg was in linseed oil. The heavy metal contents in the test samples complied with the requirements of regulatory documents for vegetable oils. An assessment of the health risk of vegetable oils with a daily consumption of 36 g per day shows that all samples of vegetable oils produced in Kazakhstan are safe for consumption. But further monitoring is needed, since all these metals are toxic and their harmful effects become apparent only after several years of exposure.

Keywords: vegetable oil, sunflower oil, linseed oil, safflower oil, toxic metals, food safety, rape oil

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Authors: Muhammad Dildar Gogi, Muhammad Arshad, Muhammad Ahsan Khan, M. Sufian, Ahmad Nawaz, Mubashir Iqbal, Muhammad Junaid Nisar, Waleed Afzal Naveed

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Larvae of silkworm (Bombyx mori) exhibit very high mortality when reared on mulberry leaves collected from mulberry orchards which get contaminated with metallic/nonmetallic compounds through either drift-deposition or chemigation. There is need to screen out such metallic compound for their toxicity at their various concentrations. The present study was carried out to assess toxicity of metals in different instars of silkworm. Aqueous solutions of nine heavy-metal based salts were prepared by dissolving 50, 100, 150, 200, 250, 300, 350 and 400 mg of each salt in one liter of water and were applied on the mulberry leaves by leaf-dip methods. The results reveal that mortality in 1st, 2nd, 3rd, 4th and 5th instar larvae caused by each heavy metal salts increased with an increase in their concentrations. The 1st instar larvae were found more susceptible to metal salts followed by 2nd, 3rd, 4th and 5th instar larvae of silkworm. Overall, Nickel chloride proved more toxic for all larval instar as it demonstrated approximately 40-99% mortality. On the basis of LC2 and larval mortality, the order of toxicity of heavy metals against all five larval instar was Nickel chloride (LC₂ = 1.9-13.9 mg/L; & 15.0±1.2-69.2±1.7% mortality) followed by Chromium nitrate (LC₂ = 3.3-14.8 mg/L; & 13.3±1.4-62.4±2.8% mortality), Cobalt nitrate (LC₂ = 4.3-30.9; &11.4±0.07-54.9±2.0% mortality), Lead acetate (LC₂ =8.8-53.3 mg/L; & 9.5±1.3-46.4±2.9% mortality), Aluminum sulfate (LC₂ = 15.5-76.6 mg/L; & 8.4±0.08-42.1±2.8% mortality), Barium sulfide (LC₂ = 20.9-105.9; & 7.7±1.1-39.2±2.5% mortality), Copper sulfate (LC2 = 28.5-12.4 mg/L; & 7.3±0.06-37.1±2.4% mortality), Manganese chloride (LC₂ = 29.9-136.9 mg/L; & 6.8±0.09-35.3±1.6% mortality) and Zinc nitrate (LC₂ = 36.3-15 mg/L; & 6.2±1.2-32.1±1.9% mortality). Zinc nitrate @ 50 and 100 mg/L, Barium sulfide @ 50 mg/L, Manganese chloride @ 50 and 100 mg/L and Copper sulfate @ 50 mg/L proved safe for 5th instar larvae as these interaction attributed no mortality. All the heavy metal salts at a concentration of 50 mg/L demonstrated less than 10% mortality.

Keywords: heavy-metals, larval-instars, lethal-concentration, mortality, silkworm

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Authors: Lakshmikanth Reddy, Bhavin Desai, Chandrakala Kari, Sanjay Sarkar, Pradeep Binu

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The sulphur dioxide gases generated as a by-product of smelting and converting operations of copper concentrate contain selenium apart from zinc, lead, copper, cadmium, bismuth, antimony, and arsenic. The gaseous stream is treated in waste heat boiler, electrostatic precipitator and scrubbers to remove coarse particulate matter in order to produce commercial grade sulfuric acid. The gas cleaning section of the acid plant uses water to scrub the smelting gases. After scrubbing, the sludge settled at the bottom of the scrubber, was analyzed in present investigation. It was found to contain 30 to 40 wt% copper and selenium up to 40 wt% selenium. The sludge collected during blow-down is directly recycled to the smelter for copper recovery. However, the selenium is expected to again vaporize due to high oxidation potential during smelting and converting, causing accumulation of selenium in sludge. In present investigation, a roasting process has been developed to recover the selenium before the copper recovery from the sludge at smelter. Selenium is associated with copper in sludge as copper selenide, as determined by X-ray diffraction and electron microscopy. The thermodynamic and thermos-gravimetry study revealed that the copper selenide phase present in the sludge was amenable to oxidation at 600°C forming oxides of copper and selenium (Cu-Se-O). However, the dissociation of selenium from the copper oxide was made possible by sulfatation using sulfur dioxide between 450 to 600°C, resulting into the formation of CuSO₄ (s) and SeO₂ (g). Lab scale trials were carried out in vertical tubular furnace to determine the optimum roasting conditions with respect to roasting time, temperature and molar ratio of O₂:SO₂. Using these optimum conditions, selenium up to 90 wt% in the form of SeO₂ vapors could be recovered from the sludge in a large-scale commercial roaster. Roasted sludge free from the selenium and containing oxides and sulfates of copper could now be recycled in the smelter for copper recovery.

Keywords: copper, selenium, copper selenide, sludge, roasting, SeO₂

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Authors: Usama Mohamed, Sam Booth, Aliysn J. Nedoma

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As part of the transition to electric vehicles, there has been a recent increase in demand for battery manufacturing. Cathodes typically account for approximately 50% of the total lithium-ion battery cell cost and are a pivotal factor in determining the viability of new industrial infrastructure. Cathodes which offer lower costs whilst maintaining or increasing performance, such as nickel-rich layered cathodes, have a significant competitive advantage when scaling up the manufacturing process. This project evaluates the techno-economic value proposition of an integrated industrial scale cathode active material (CAM) production process, closing the mass and energy balances, and optimizing the operation conditions using a sensitivity analysis. This is done by developing a process model of a co-precipitation synthesis route using Aspen Plus software and validated based on experimental data. The mechanism chemistry and equilibrium conditions were established based on previous literature and HSC-Chemistry software. This is then followed by integrating the energy streams, adding waste recovery and treatment processes, as well as testing the effect of key parameters (temperature, pH, reaction time, etc.) on CAM production yield and emissions. Finally, an economic analysis estimating the fixed and variable costs (including capital expenditure, labor costs, raw materials, etc.) to calculate the cost of CAM ($/kg and $/kWh), total plant cost ($) and net present value (NPV). This work sets the foundational blueprint for future research into sustainable industrial scale processes for CAM manufacturing.

Keywords: cathodes, industrial production, nickel-rich layered cathodes, process modelling, techno-economic analysis

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Authors: Jaime Pizarro, Ximena Castillo

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The intensive use of water in agriculture, industry, human consumption and increasing pollution are factors that reduce the availability of water for future generations; the challenge is to advance in sustainable and low-cost solutions to reuse water and to facilitate the availability of the resource in quality and quantity. The use of new low-cost materials with sorbent capacity for pollutants is a solution that contributes to the improvement and expansion of water treatment and reuse systems. Fly ash, a residue from the combustion of coal in power plants that is produced in large quantities in newly industrialized countries, contains a high amount of silicon oxides and aluminum oxides, whose properties can be used for the synthesis of mesoporous materials. Properly functionalized, this material allows obtaining matrixes with high sorption capacity. The mesoporous materials have a large surface area, thermal and mechanical stability, uniform porous structure, and high sorption and functionalization capacities. The goal of this study was to develop hexagonal mesoporous siliceous material (HMS) for the adsorption of sulphate from industrial and mining waters. The silica was extracted from fly ash after calcination at 850 ° C, followed by the addition of water. The mesoporous structure has a surface area of 282 m2 g-1 and a size of 5.7 nm and was functionalized with ethylene diamine through of a self-assembly method. The material was characterized by Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS). The capacity of sulphate sorption was evaluated according to pH, maximum load capacity and contact time. The sulphate maximum adsorption capacity was 146.1 mg g-1, which is three times higher than commercial sorbents. The kinetic data were fitted according to a pseudo-second order model with a high coefficient of linear regression at different initial concentrations. The adsorption isotherm that best fitted the experimental data was the Freundlich model.

Keywords: fly ash, mesoporous siliceous, sorption, sulphate

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Authors: Marc Evenst Jn Jacques, Sophie Bernard

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Electrical and electronic applications, as well as rechargeable batteries, are common in any economy. They also contain a number of important and valuable metals. It is critical to investigate the impact of these new materials or volume sources on the metal market dynamics. This paper investigates the impact of responsible recycling within the European region on metal price volatility. As far as we know, no empirical studies have been conducted to assess the role of metal recycling in metal market price volatility. The goal of this paper is to test the claim that metal recycling helps to cushion price volatility. A set of circular economy indicators/variables, namely, 1) annual total trade values of recycled metals, 2) annual volume of scrap traded and 3) circular material use rate, and 4) information about recycling, are used to estimate the volatility of monthly spot prices of regular metals. A combination of the GARCH-MIDAS model for mixed frequency data sampling and a simple GARCH (1,1) model for the same frequency variables was adopted to examine the potential links between each variable and price volatility. We discovered that from 2010 to 2019, except for Nickel, scrap consumption (Millions of tons), Scrap Trade Values, and Recycled Material use rate had no significant impact on the price volatility of standard metals (Aluminum, Lead) and precious metals (Gold and Platinum). Worldwide interest in recycling has no impact on returns or volatility. Specific interest in metal recycling did have a link to the mean return equation for Aluminum, Gold and to the volatility equation for lead and Nickel.

Keywords: recycling, circular economy, price volatility, GARCH, mixed data sampling

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Authors: Hasan Izhar Khan, Naiqiang Zhang, Hong Xu, Zhongliang Zhu, Dongfang Jiang

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Inconel 625 is a nickel-based alloy having outstanding corrosion resistance and developed for use at service temperatures ranging from cryogenic to 980°C. It got a wide range of applications in nuclear, petrochemical, chemical, marine, aeronautical, and aerospace industries. Currently, it is one of the candidate materials to be used as a structural material in ultra-supercritical (USC) power plants. In the high-temperature corrosive medium environment, metallic materials are susceptible to corrosion fatigue (CF). CF is an interaction between cyclic stress and corrosive medium environment that acts on a susceptible material and results in initiation and propagation of cracks. For the application of Inconel 625 as a structural material in USC power plants, CF behavior must be evaluated in steam and supercritical water (SCW) environment. Fatigue crack growth rate (FCGR) curves obtained from CF experiments are required to predict residual life of metallic materials used in power plants. In this study, FCGR tests of Inconel 625 were obtained by using compact tension specimen at 550-650 °C in steam (8 MPa) and SCW (25 MPa). The dissolved oxygen level was kept constant at 8000 ppb for the test conducted in steam and SCW. The tests were performed under sine wave loading waveform, 1 Hz loading frequency, stress ratio of 0.6 and maximum stress intensity factor of 32 MPa√m. Crack growth rate (CGR) was detected by using direct current potential drop technique. Results showed that CGR increased with an increase in temperature in the tested environmental conditions. The mechanism concerning the influence of temperature on FCGR are further discussed.

Keywords: corrosion fatigue, crack growth rate, nickel-based alloy, temperature

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Authors: Remy Mpulumba Badiambile, Paul Musa Obadia, Malick Useni Mutayo, Jeef Numbi Mukanya, Patient Nkulu Banza, Tony Kayembe Kitenge, Erik Smolders, Jean-François Picron, Vincent Haufroid, Célestin Banza Lubaba Nkulu, Benoit Nemery

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Background: In July 2021, the Tshikapa river became heavily polluted by mining wastes from a diamond mine in neighboring Angola, leading to massive killing of fish, as well as disease and even deaths among residents living along the Tshikapa and Kasai rivers, a major contributory of the Congo river. The exact nature of the pollutants was unknown. Methods: In a cross-sectional study conducted in the city of Tshikapa in August 2021, we enrolled by opportunistic sampling 65 residents (11 children < 16y) living alongside the polluted rivers and 65 control residents (5 children) living alongside a non-affected portion of the Kasai river (upstream from the Tshikapa-Kasai confluence). We administered a questionnaire and obtained spot urine samples for measurements of thiocyanate (a metabolite of cyanide) and 26 trace metals (by ICP-MS). Metals (and pH) were also measured in samples of river water. Results: Participants from both groups consumed river water. In the area affected by the pollution, most participants had eaten dead fish. Prevalences of reported health symptoms were higher in the exposed group than among controls: skin rashes (52% vs 0%), diarrhea (40% vs 8%), abdominal pain (8% vs 3%), nausea (3% vs 0%). In polluted water, concentrations [median (range)] were only higher for nickel [(2.2(1.4–3.5)µg/L] and uranium [78(71–91)ng/L] than in non-polluted water [0.8(0.6–1.9)µg/L; 9(7–19)ng/L]. In urine, concentrations [µg/g creatinine, median(IQR)] were significantly higher in the exposed group than in controls for lithium [19.5(12.4–27.3) vs 6.9(5.9–12.1)], thallium [0.41(0.31–0.57) vs 0.19(0.16–0.39)], and uranium [0.026(0.013–0.037)] vs 0.012(0.006–0.024)]. Other elements did not differ between the groups, but levels were higher than reference values for several metals (including manganese, cobalt, nickel, and lead). Urinary thiocyanate concentrations did not differ. Conclusion: This study, after an ecological disaster in the DRC, has documented contamination of river water by nickel and uranium and high urinary levels of some trace metals among affected riverine populations. However, the exact cause of the massive fish kill and disease among residents remains elusive. The capacity to rapidly investigate toxic pollution events must be increased in the area.

Keywords: metal contaminants, river water and human urine, pollution by mining wastes, DR Congo

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Authors: Adilah Shariff, Nurhidayah Mohamed Noor, Alexander Lau, Muhammad Azwan Mohd Ali

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Biomass such as corn and cassava wastes if left to decay will release significant quantities of greenhouse gases (GHG) including carbon dioxide and methane. The biomass wastes can be converted into biochar via thermochemical process such as slow pyrolysis. This approach can reduce the biomass wastes as well as preserve its carbon content. Biochar has the potential to be used as a carbon sequester and soil amendment. The aim of this study is to investigate the characteristics of the corn cob, cassava stem, and cassava rhizome in order to identify their potential as pyrolysis feedstocks for biochar production. This was achieved by using the proximate and elemental analyses as well as calorific value and lignocellulosic determination. The second objective is to investigate the effect of pyrolysis temperature on the biochar produced. A fixed bed slow pyrolysis reactor was used to pyrolyze the corn cob, cassava stem, and cassava rhizome. The pyrolysis temperatures were varied between 400 °C and 600 °C, while the heating rate and the holding time were fixed at 5 °C/min and 1 hour, respectively. Corn cob, cassava stem, and cassava rhizome were found to be suitable feedstocks for pyrolysis process because they contained a high percentage of volatile matter more than 80 mf wt.%. All the three feedstocks contained low nitrogen and sulphur content less than 1 mf wt.%. Therefore, during the pyrolysis process, the feedstocks give off very low rate of GHG such as nitrogen oxides and sulphur oxides. Independent of the types of biomass, the percentage of biochar yield is inversely proportional to the pyrolysis temperature. The highest biochar yield for each studied temperature is from slow pyrolysis of cassava rhizome as the feedstock contained the highest percentage of ash compared to the other two feedstocks. The percentage of fixed carbon in all the biochars increased as the pyrolysis temperature increased. The increment of pyrolysis temperature from 400 °C to 600 °C increased the fixed carbon of corn cob biochar, cassava stem biochar and cassava rhizome biochar by 26.35%, 10.98%, and 6.20% respectively. Irrespective of the pyrolysis temperature, all the biochars produced were found to contain more than 60 mf wt.% fixed carbon content, much higher than its feedstocks.

Keywords: biochar, biomass, cassava wastes, corn cob, pyrolysis

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Authors: Aurore Lechevallier, Mohend Chaouche, Jerome Soudier, Guillaume Renaudin

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The cement industry accounts for 8% of the global CO₂ emissions, and approximately 60% of these emissions are associated with the Portland cement clinker production from the decarbonization of limestone (CaCO3). Their impact on the greenhouse effect results in growing social awareness. Therefore, CO2 footprint becomes a product selection choice, and substituting Portland cement with a lower CO2-footprint alternative binder is sought. In this context, new hydraulic binders have been studied as a potential Ordinary Portland Cement substitute. Many of them are composed of iron oxides and aluminum oxides, present in the Ca₄Al₂-xFe₂+ₓO₁₀-like phase and forming Ca-LDH (i.e. AFM) as a hydration product. It has become essential to study the possible existence of Fe/Al AFM solid solutions to characterize the hydration process properly. Ca₂Al₂-xFex(OH)₆.X.nH₂O layered AFM samples intercalated with either nitrate or chloride X anions were synthesized based on the co-precipitation method under a nitrogen atmosphere to avoid the carbonation effect.AFM samples intercalated with carbonate anions were synthesized based on the anionic exchange process, using AFM-NO₃ as the source material. These three AFM samples were synthesized with varying Fe/Al molar ratios. The experimental conditions were optimized to make possible the formation of Al-AFM and Fe-AFM using the same parameters (namely pH value and salt concentration). Rietveld refinements were performed to demonstrate the existence of a solid solution between the two trivalent metallic end members. Spectroscopic analyses were used to confirm the intercalation of the targeted anion; secondary electron images were taken to analyze the AFM samples’ morphology, and energy dispersive X-ray spectroscopy (EDX) was carried out to determine the elemental composition of the AFM samples. Results of this study make it possible to quantify the Al/Fe ratio of the AFM phases precipitated in our hydraulic binder, thanks to the determined Vegard's law characteristic to the corresponding solid solutions

Keywords: AFm phase, iron-rich binder, low-carbon cement, solid solution

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Authors: Fiona S. Motswaiso, Kengo Nakamura, Takeshi Komai

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Heavy metals may occur naturally in rocks and soils, but elevated quantities of them are being gradually released into the environment by anthropogenic activities such as mining. In order to address issues of heavy metal water and soil pollution, a distinction needs to be made between natural and anthropogenic anomalies. The current study aims at characterizing the spatial distribution of trace elements and evaluate site-specific geochemical background concentrations of trace elements in the mine soils examined, and also to discriminate between lithogenic and anthropogenic sources of enrichment around a copper-nickel mining town in Selibe-Phikwe, Botswana. A total of 20 Soil samples, 11 river sediment, and 9 river water samples were collected from an area of 625m² within the precincts of the mine and the smelter. The concentrations of metals (Cu, Ni, Pb, Zn, Cr, Ni, Mn, As, Pb, and Co) were determined by using an ICP-MS after digestion with aqua regia. Major elements were also determined using ED-XRF. Water pH and EC were measured on site and recorded while soil pH and EC were also determined in the laboratory after performing water elution tests. The highest Cu and Ni concentrations in soil are 593mg/kg and 453mg/kg respectively, which is 3 times higher than the crustal composition values and 2 times higher than the South African minimum allowable levels of heavy metals in soils. The level of copper contamination was higher than that of nickel and other contaminants. Water pH levels ranged from basic (9) to very acidic (3) in areas closer to the mine/smelter. There is high variation in heavy metal concentration, eg. Cu suggesting that some sites depict regional natural background concentrations while other depict anthropogenic sources.

Keywords: contamination, geochemical baseline, heavy metals, soils

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Authors: Siba Soren, Purnendu Parhi

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Today, the world is facing a severe challenge due to depletion of traditional fossil fuels. Scientists across the globe are working for a solution that involves a dramatic shift to practical and environmentally sustainable energy sources. High-capacity energy systems, such as metal-air batteries, fuel cells, are highly desirable to meet the urgent requirement of sustainable energies. Among the fuel cells, Direct methanol fuel cells (DMFCs) are recognized as an ideal power source for mobile applications and have received considerable attention in recent past. In this advanced electrochemical energy conversion technologies, Oxygen Reduction Reaction (ORR) is of utmost importance. However, the poor kinetics of cathodic ORR in DMFCs significantly hampers their possibilities of commercialization. The oxygen is reduced in alkaline medium either through a 4-electron (equation i) or a 2-electron (equation ii) reduction pathway at the cathode ((i) O₂ + 2H₂O + 4e⁻ → 4OH⁻, (ii) O₂ + H₂O + 2e⁻ → OH⁻ + HO₂⁻ ). Due to sluggish ORR kinetics the ability to control the reduction of molecular oxygen electrocatalytically is still limited. The electrocatalytic ORR starts with adsorption of O₂ on the electrode surface followed by O–O bond activation/cleavage and oxide removal. The reaction further involves transfer of 4 electrons and 4 protons. The sluggish kinetics of ORR, on the one hand, demands high loading of precious metal-containing catalysts (e.g., Pt), which unfavorably increases the cost of these electrochemical energy conversion devices. Therefore, synthesis of active electrocatalyst with an increase in ORR performance is need of the hour. In the recent literature, there are many reports on transition metal oxide (TMO) based ORR catalysts for their high activity TMOs are also having drawbacks like low electrical conductivity, which seriously affects the electron transfer process during ORR. It was found that 2D graphene layer is having high electrical conductivity, large surface area, and excellent chemical stability, appeared to be an ultimate choice as support material to enhance the catalytic performance of bare metal oxide. g-C₃N₄ is also another candidate that has been used by the researcher for improving the ORR performance of metal oxides. This material provides more active reaction sites than other N containing carbon materials. Rare earth oxide like CeO₂ is also a good candidate for studying the ORR activity as the metal oxide not only possess unique electronic properties but also possess catalytically active sites. Here we will discuss the ORR performance (in alkaline medium) of N-rGO/C₃N₄ supported nano Cerium Oxides hybrid synthesized by microwave assisted Solvothermal method. These materials exhibit superior electrochemical stability and methanol tolerance capability to that of commercial Pt/C.

Keywords: oxygen reduction reaction, electrocatalyst, cerium oxide, graphene

Procedia PDF Downloads 156