Search results for: crystalline silica

Authors: Gonzalo Ortiz de Elguea-Culebras, Raúl Sánchez-Vioquea, Adela Mena-Morales, Manuel Alaiz, Enrique Melero-Bravo, Esteban García-Romero, Javier Vioque, Lourdes Marchante-Cuevas, Julio Girón-Calle

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Saffron (Crocus sativus L.) is a highly valued crop for the manufacture of spice that consists of the dried stigma of the flowers. This is in contrast to other underutilized parts of the saffron plant as leaves, which represent abundant biomass whose use might help to enhance the sustainability of the saffron crop. Saffron leaves contain significant amounts of phenolic compounds, 7.8 equivalent grams of gallic acid per 100g of extract, and are very promising compounds in terms of exploring novel uses of saffron leaves. Given that phenolic compounds have numerous effects on cancer-related biological pathways, we have investigated the in vitro antiproliferative effect of saffron leaf polyphenols against human colon adenocarcinoma cells (Caco-2). Polyphenols were extracted from leaves with 70% ethanol, defatted with hexane, and purified by solid phase extraction using C18 silica gel and then silica gel 60. Analysis of polyphenols was performed by HPLC-ESI-MS. Di-, tri-, and tetrahexosides of quercetin, kaempferol, and isorhamnetin, as well as C-hexosides like isoorientin and vitexin, were tentatively identified. Polyphenols strongly inhibited the proliferation of Caco-2 cells, which is consistent with model studies in which several of the polyphenols identified in saffron leaves have demonstrated their potential as chemopreventive agents in cancer. Due to the low profitability that saffron leaf currently represents, we consider these results very encouraging and that this by-product deserves further investigation as a potential source of active molecules against colorectal cancer.

Keywords: saffron leaves, agricultural by-products, polyphenols, antiproliferative effect, human colon adenocarcinoma cells

Procedia PDF Downloads 95

Authors: Chris Miskelly, Eoin Cunningham, Beatrice Smyth, John. D. Holbrey, Gosia Swadzba-Kwasny, Emily L. Byrne, Yoan Delavoux, Mantian Li.

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Recently, the use of ionic liquids (ILs) for the preparation of lignocellulose derived cellulosic materials as alternatives to petrochemical feedstocks has been the focus of considerable research interest. While the technical viability of IL-based lignocellulose treatment methodologies has been well established, the high cost of reagents inhibits commercial feasibility. This work aimed to assess the technoeconomic viability of the preparation of cellulose rich materials (CRMs) using protic ionic liquids (PILs) synthesized from low cost alkylamines and sulphuric acid. For this purpose, the tertiary alkylamines, triethylamine, and dimethylbutylamine were selected. Bulk scale production cost of the synthesized PILs, triethylammonium hydrogen sulphate and dimetheylbutylammonium hydrogen sulphate, was reported as $0.78 kg-1 to $1.24 kg-1. CRMs were prepared through the treatment of common wheat (Triticum aestivum) straw with these PILs. By controlling treatment parameters, CRMs with a cellulose content of ≥ 80 wt% were prepared. This was achieved using a T. aestivum straw to PIL loading ratio of 1:15 w/w, a treatment duration of 180 minutes, and ethanol as a cellulose antisolvent. Infrared spectra data and decreased onset degradation temperature of CRMs (ΔTONSET ~ 70 °C) suggested the formation of cellulose sulphate esters during treatment. Chemical derivatisation can aid the dispersion of prepared CRMs in non-polar polymer/ composite matrices, but act as a barrier to thermal processing at temperatures above 150 °C. It was also shown that treatment increased the crystallinity of CRMs (ΔCrI ~ 40 %) without altering the native crystalline structure or crystallite size (~ 2.6 nm) of cellulose; peaks associated with the cellulose I crystalline planes (110), (200), and (004) were observed at Bragg angles 16.0 °, 22.5 ° and 35.0 ° respectively. This highlighted the inability of assessed PILs to dissolve crystalline cellulose and was attributed to the high acidity (pKa ~ - 1.92 to - 6.42) of sulphuric acid derived anions. Electron micrographs revealed that the stratified multilayer tissue structure of untreated T. aestivum straw was significantly modified during treatment. T. aestivum straw particles were disassembled during treatment, with prepared CRMs adopting a golden-brown film-like appearance. This work demonstrated the degradation of non-cellulosic fractions of lignocellulose without dissolution of cellulose. It is the first to report on the derivatisation of cellulose during treatment with protic hydrogen sulphate ionic liquids, and the potential implications of this with reference to biopolymer feedstock preparation.

Keywords: cellulose, extraction, protic ionic liquids, esterification, thermal stability, waste valorisation, biopolymer feedstock

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Authors: Atef Y. Shenouda, Anton A. Momchilov

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Graphene and CdO with different stoichiometric ratios of Cd(CH₃COO)₂ and graphene samples were prepared by hydrothermal reaction. The crystalline phases of pure CdO and 3CdO:1graphene were identified by X-ray diffraction (XRD). The particle morphology was studied with SEM. Furthermore, impedance measurements were applied. Galvanostatic measurements for the cells were carried out using potential limits between 0.01 and 3 V vs. Li/Li⁺. The current cycling intensity was 10⁻⁴ A. The specific discharge capacity of 3CdO-1G cell was about 450 Ah.Kg⁻¹ up to more than 100 cycles.

Keywords: CdO, graphene, negative electrode, lithium battery

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Authors: E. Gandomkar, S. Sabbaghi

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In this paper, the effects of variation synthesized methods on morphology and size of silica nanostructure via modifying sol-gel and precipitation method have been investigated. Meanwhile, resulting products have been characterized by particle size analyzer, scanning electron microscopy (SEM), X-ray Diffraction (XRD) and Fourier transform infrared (FT-IR) spectra. As result, the shape of SiO2 with sol-gel and precipitation methods was spherical but with modifying sol-gel method we have been had nanolayer structure.

Keywords: modified sol-gel, precipitation, nanolayer, Na2SiO3, nanoparticle

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Authors: Mutwakil Nafi, Abed Elaziz El Amein, Muna El Dawi, Khalafala Salih, Osma Elbahi, Abed Elhalim Abou

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Recently a large deposit of oolitic iron ore of Late Carboniferous-Permotriassic-Lower Jurassic age was discovered in Wadi Halfa and Argein areas, North Sudan. It seems that the iron ore mineralization exists in the west and east bank of the River Nile of the study area that are found on the Egyptian-Sudanese border. The Carboniferous-Lower Jurassic age strata were covered by 67 sections and each section has been examined and carefully described. The iron-ore in Wadi Halfa occurs as oolitic ironstone and contained two horizons: (A) horizon and (B) horizon. Only horizon (A) was observed in southern Argein area. The texture of the ore is variable depending on the volume of the component. In thin sections the average of the ooids were ranged between 90% - 80%. The matrix varies between 10%-20% by volume and detritus quartz in other component my reach up to 30% by volume in sandy massive ore. Ooids size ranges from 0.2mm-1.00 mm on average in very coarse ooids may attend up to 1 mm in size. The matrix around the ooids is dominated by iron hydroxide, carbonate, fine and amorphous silica. The probable ore reserve estimate of 1.234 billion at a head grade of 41.29% Fe for the Wadi Halfa Oolitic Ironstone Formation. The iron ore shows higher content of phosphorus ranges from 6.15% to 0.16%, with mean 1.45%. The new technology Hatch–Ironstone Chloride Segregation (HICS) can be used to produce commercial-quality of iron and reduce phosphorus and silica to acceptable levels for steel industry. The development of infra structures and presence huge quantity of iron ore would make exploitation of the iron ore economic.

Keywords: HICS, Late Carboniferous age, oolitic iron ore, phosphorus

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Authors: Milton Manyangadze, Joseph Govha, T. Bala Narsaiah, Ch. Shilpa Chakra

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The availability and access to fresh water is today a serious global challenge. This has been a direct result of factors such as the current rapid industrialization and industrial growth, persistent droughts in some parts of the world, especially in the sub-Saharan Africa as well as population growth. Growth of the chemical processing industry has also seen an increase in the levels of pollutants in our water bodies which include heavy metals among others. Heavy metals are known to be dangerous to both human and aquatic life. As such, they have been linked to several diseases. This is mainly because they are highly toxic. They are also known to be bio accumulative and non-biodegradable. Lead for example, has been linked to a number of health problems which include damage of vital internal body systems like the nervous and reproductive system as well as the kidneys. From this background therefore, the removal of the toxic heavy metal, Pb2+ from waste water was investigated using nano silica hollow spheres (NSHS) as the adsorbent. Synthesis of NSHS was done using a three-stage process in which CaCO3 nanoparticles were initially prepared as a template. This was followed by treatment of the formed oxide particles with NaSiO3 to give a nanocomposite. Finally, the template was destroyed using 2.0M HCl to give NSHS. Characterization of the nanoparticles was done using analytical techniques like XRD, SEM, and TGA. For the adsorption process, both thermodynamic and equilibrium studies were carried out. Thermodynamic studies were carried out and the Gibbs free energy, Enthalpy and Entropy of the adsorption process were determined. The results revealed that the adsorption process was both endothermic and spontaneous. Equilibrium studies were also carried out in which the Langmuir and Freundlich isotherms were tested. The results showed that the Langmuir model best described the adsorption equilibrium.

Keywords: characterization, endothermic, equilibrium studies, Freundlich, Langmuir, nanoparticles, thermodynamic studies

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Authors: Eric Noe Hernandez Rodriguez, Cristian Esneider Penuela Cruz

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Magnesium is a biocompatible and biodegradable material that has gained increased interest for application in resorbable orthopedic implants. However, to date, much research is being conducted to overcome the main disadvantage: its low corrosion resistance. In this work, we report our findings on the development and application of TiO₂-MgO coatings to improve and modulate the corrosion resistance of magnesium pieces. The plasma electrolytic oxidation (PEO) technique was employed to obtain the TiO₂-MgO coatings. The effect of the experimental parameters on the modulation of the TiO₂:MgO ratio was investigated. The most critical parameters were the chemical composition of the precursor electrolytic solution and the current density. According to scanning electron microscopy (SEM) observations, the coatings were porous; however, they become more compact as the current density increases. XRD measurements showed that the coatings are formed by a composite consisting of TiO₂ and MgO oxides, whose ratio can be changed by the experimental conditions. TiO₂ had the anatase crystalline structure, while the MgO had the FCC crystalline structure. The corrosion resistance was evaluated through the corrosion current (Icorr) measured at room temperature by the polarization technique (Tafel). For doing it, Hank's solution was used in order to simulate the body fluids. Also, immersion tests were conducted. Tafel curves showed an improvement of the corrosion resistance at some coated magnesium pieces in contrast to control pieces (uncoated). Corrosion currents were lower, and the corrosion potential changed to positive values. It was observed that the experimental parameters allowed to modulate the protective capacity of the coatings by changing the TiO₂:MgO ratio. Coatings with a higher content of TiO₂ (measured by energy dispersive spectroscopy) showed higher corrosion resistance. Results showed that TiO₂-MgO coatings can be successfully applied to improve the corrosion resistance of Mg pieces in simulated body fluid; even more, the corrosion resistance can be tuned by changing the TiO₂:MgO ratio.

Keywords: biomaterials, PEO, corrosion resistance, magnesium

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Authors: Ali Mohammed Yimer, Ayalew H. Assen, Youssef Belmabkhout

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This study delves into sustainable approaches for valorizing phosphatic wastes, specifically phosphate mining wastes and phosphogypsum, which are byproducts of phosphate industries and pose significant environmental challenges due to their accumulation. We propose a unified strategic synthesis method aimed at converting these wastes into hetero-functional porous materials. Our approach involves isolating the primary components of phosphatic wastes, such as CaO, SiO2 and Al2O3 to fabricate functional porous materials falling into two distinct classes. Firstly, alumina and silica components are extracted or isolated to produce zeolites (including CAN, GIS, SOD, FAU, and LTA), characterized by a Si/Al ratio of less than 5. Secondly, residual calcium is utilized to synthesize calcium-based metal–organic frameworks (Ca-MOFs) employing various organic linkers like Ca-BDC, Ca-BTC and Ca-TCPB (SBMOF-2), thereby providing flexibility in material design. Characterization techniques including XRD, SEM-EDX, FTIR, and TGA-MS affirm successful material assembly, while sorption analyses using N2, CO2, and H2O demonstrate the porosity of the materials. Particularly noteworthy is the water/alcohol separation potential exhibited by the Ca-BTC MOF, owing to its optimal pore aperture size (∼3.4 Å). To enhance replicability and scalability, detailed protocols for each synthesis step and specific conditions for each process are provided, ensuring that the methodology can be easily reproduced and scaled up for industrial applications. This synthetic transformation approach represents a valorization route for converting phosphatic wastes into extended porous structures, promising significant environmental and economic benefits.

Keywords: calcium-based metal-organic frameworks, low-silica zeolites, porous materials, sustainable synthesis, valorization

Procedia PDF Downloads 38

Authors: Tatiana L. Avalos-Rendon, Elias A. Pasten Chelala, Carlos J. Mendoza EScobedo, Ignacio A. Figueroa, Victor H. Lara, Luis M. Palacios-Romero

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The cement industry is facing cost increments in energy supply, requirements for reduction of CO₂, and insufficient supply of raw materials of good quality. According to all these environmental issues, cement industry must change its consumption patterns and reduce CO₂ emissions to the atmosphere. This can be achieved by generating environmental consciousness, which encourages the use of industrial by-products and/or recycling for the production of cement, as well as alternate, environment-friendly methods of synthesis which reduce CO₂. Calcination is the conventional method for the obtainment of Portland cement clinker. This method consists of grinding and mixing of raw materials (limestone, clay, etc.) in an adequate dosage. Resulting mix has a clinkerization temperature of 1450 °C so that the formation of the main component occur: alite (Ca₃SiO₅, C₃S). Considering that the energy required to produce C₃S is 1810 kJ kg -1, calcination method for the obtainment of clinker represents two major disadvantages: long thermal treatment and elevated temperatures of synthesis, both of which cause high emissions of carbon dioxide (CO₂) to the atmosphere. Belite Portland clinker is characterized by having a low content of calcium oxide (CaO), causing the presence of alite to diminish and favoring the formation of belite (β-Ca₂SiO₄, C₂S), so production of clinker requires a reduced energy consumption (1350 kJ kg-1), releasing less CO₂ to the atmosphere. Conventionally, β-Ca₂SiO₄ is synthetized by the calcination of calcium carbonate (CaCO₃) and silicon dioxide (SiO₂) through the reaction in solid state at temperatures greater than 1300 °C. Resulting belite shows low hydraulic reactivity. Therefore, this study concerns a new simple modified combustion method for the synthesis of two belite cements at low temperatures (1000 °C). Silica fume, as subproduct of metallurgic industry and commercial natural zeolite were utilized as raw materials. These are considered low-cost materials and were utilized with no additional purification process. Belite cements properties were characterized by XRD, SEM, EDS and BET techniques. Hydration capacity of belite cements was calculated while the mechanical strength was determined in ordinary Portland cement specimens (PC) with a 10% partial replacement of the belite cements obtained. Results showed belite cements presented relatively high surface áreas, at early ages mechanical strengths similar to those of alite cement and comparable to strengths of belite cements obtained by different synthesis methods. Cements obtained in this work present good hydraulic reactivity properties.

Keywords: belite, silica fume, zeolite, hydraulic reactivity

Procedia PDF Downloads 347

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: N. Stoeva, I. Spassova, R. Nickolov, M. Khristova

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Exhaust gases from stationary and mobile combustion sources contain nitrogen oxides that cause a variety of environmentally harmful effects. The most common approach of their elimination is the catalytic reaction in the exhaust using various reduction agents such as NH3, CO and hydrocarbons. Transition metals (Co, Ni, Cu, etc.) are the most widely used as active components for deposition on various supports. However, since the interaction between different catalyst components have been extensively studied in different types of reaction systems, the possible cooperation between active components and the support material and the underlying mechanisms have not been thoroughly investigated. The support structure may affect how these materials maintain an active phase. The objective is to investigate the addition of carbonaceous materials with different nature and texture characteristics on the properties of the resulting silica-carbon support and how it influences of the catalytic properties of the supported copper and cobalt catalysts for reduction of NO with CO. The versatility of the physico-chemical properties of the composites and the supported copper and cobalt catalysts are discussed with an emphasis on the relationship of the properties with the catalytic performance. The catalysts were prepared by sol-gel process and were characterized by XRD, XPS, AAS and BET analysis. The catalytic experiments were carried out in catalytic flow apparatus with isothermal flow reactor in the temperature range 20–300оС. After the catalytic test temperature-programmed desorption (TPD) was carried out. The transient response method was used to study the interaction of the gas phase with the catalyst surface. The role of the interaction between the support and the active phase on the catalyst’s activity in the studied reaction was discussed. We suppose the carbon particles with small sizes to participate in the formation of the active sites for the reduction of NO with CO along with their effect on the kind of deposited metal oxide phase. The existence of micropore texture for some of composites also influences by mass-transfer limitations.

Keywords: catalysts, no reduction, composites, bet analysis

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Authors: A. Kabir, D. Boulainine, I. Bouanane, N. Benslim, B. Boudjema, C. Sedrati

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SnO₂ is an n-type semiconductor with a direct gap of about 3.6 eV. It is largely used in several domains such as nanocrystalline photovoltaic cells. Due to its interesting physic-chemical properties, this material was elaborated in thin film forms using different deposition techniques. It was found that SnO₂ properties were directly affected by the deposition method parameters. In this work, the RGTO method (Rheotaxial Growth and Thermal Oxidation) was used to deposit elaborate SnO₂ thin films. This technique consists on thermal oxidation of the Sn films deposited onto a substrate heated to a temperature close to Sn melting point (232°C). Such process allows the preparation of high porosity tin oxide films which are very suitable for the gas sensing. The films structural, morphological and optical properties pre and post thermal oxidation were studied using X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-Visible spectroscopy and Fourier transform infrared spectroscopy (FTIR) respectively. XRD patterns showed a polycrystalline structure of the cassiterite phase of SnO₂. The grain growth was found affected by the oxidation temperature. This grain size evolution was confronted to existing grain growth models in order to understand the growth mechanism. From SEM images, the as deposited Sn film was formed of difference diameter spherical agglomerations. As a function of the oxidation temperature, these spherical agglomerations shape changed due to the introduction of oxygen ions. The deformed spheres started to interconnect by forming bridges between them. The volume porosity, determined from the UV-Visible reflexion spectra, Changes as a function of the oxidation temperature. The variation of the crystalline fraction, determined from FTIR spectra, correlated with the variation of both the grain size and the volume porosity.

Keywords: tin oxide, RGTO, grain growth, volume porosity, crystalline fraction

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Authors: Anna Strakowska, Marian Zaborski

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This abstract focuses an overview of the methods used to create self-healing silicone composites. It has been shown how incorporating of polyhedral oligomeric silsesquioxanes (POSS) molecules with acid and basic groups to silicone rubber affects the barrier properties, mechanical properties in room and reduced temperature or the influence on relaxation rates of the methylvinylsilicone rubber vulcanizates. Moreover, the presence of silsesquioxanes, their content and the way of composites preparing affect the amount of ionic bonds, as indicated by dynamic - mechanical thermal analysis (DMTA) as well as measurements of equilibrium swelling in toluene. The aim of this work was to study the influence of concentration and different functional groups types selected silsesquioxanes compounds on self-healing effect of silicone rubber and obtain elastomers with good barrier and mechanical properties. Composites based on the methylvinylsilicone rubber with fumed silica as the fillers were manufactured and studied. To obtain self-healing effect various silsesquioxanes with amino and acid groups were used. Every tested sample demonstrated the ability to the self-treatment. The most significant effect was observed for system containing amic-acid isobytyl POSS/ aminopropylisobutyl POSS. Composite with this silsesquioxanes was exhibited the best improvement of gas permeability after heal. Moreover, the addition of POSS with acid and basic groups clearly affects the mechanical properties of the vulcanizates. The most significant effect was observed for the composite material consisting of amic-acid isobytyl POSS / aminoethylaminopropylisobutyl POSS, which tensile strength was even greater than the reference vulcanizate with fumed silica. The development of autonomous self-healing materials could have an enormous influence on all industry branches from motorization to power industry. Self-repairing materials would have a massive impact on lengthening product lifetimes, increasing safety, and lowering product costs by reducing maintenance requirements.

Keywords: barrier properties, mechanical properties, POSS, self-healing composites

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Authors: Ergin Kosa, Ali Göksenli

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Erosion and abrasion are wear mechanisms reducing the lifetime of machine elements like valves, pump and pipe systems. Both wear mechanisms are acting at the same time, causing a “Synergy” effect, which leads to a rapid damage of the surface. Different parameters are effective on erosive abrasive wear rate. In this study effect of particle impact angle on wear rate and wear mechanism of ductile and brittle materials was investigated. A new slurry pot was designed for experimental investigation. As abrasive particle, silica sand was used. Particle size was ranking between 200-500 µm. All tests were carried out in a sand-water mixture of 20% concentration for four hours. Impact velocities of the particles were 4,76 m/s. As ductile material steel St 37 with Brinell Hardness Number (BHN) of 245 and quenched St 37 with 510 BHN was used as brittle material. After wear tests, morphology of the eroded surfaces were investigated for better understanding of the wear mechanisms acting at different impact angles by using optical microscopy and Scanning Electron Microscope. The results indicated that wear rate of ductile material was higher than brittle material. Maximum wear was observed by ductile material at a particle impact angle of 300. On the contrary wear rate increased by brittle materials by an increase in impact angle and reached maximum value at 450. High amount of craters were detected after observation on ductile material surface Also plastic deformation zones were detected, which are typical failure modes for ductile materials. Craters formed by particles were deeper according to brittle material worn surface. Amount of craters decreased on brittle material surface. Microcracks around craters were detected which are typical failure modes of brittle materials. Deformation wear was the dominant wear mechanism on brittle material. At the end it is concluded that wear rate could not be directly related to impact angle of the hard particle due to the different responses of ductile and brittle materials.

Keywords: erosive wear, particle impact angle, silica sand, wear rate, ductile-brittle material

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Authors: Sabriye Piskin, Sibel Kasap, Muge Sari Yilmaz

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Nanocrystalline TiO₂ particles were successfully synthesized via sol-gel and sonochemical combination using titanium tetraisopropoxide as a precursor at lower temperature for a short time. The effect of the reaction parameters (hydrolysis media, acid media, and reaction temperatures) on the synthesis of TiO₂ particles were investigated in the present study. Characterizations of synthesized samples were prepared by X-ray diffraction (XRD) analysis. It was shown that the reaction parameters played a significant role in the synthesis of TiO₂ particles.

Keywords: crystalline TiO2, sonochemical mechanism, sol-gel reaction, XRD

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Authors: C. Nakib, N. Ammouchi, A. Otmani, A. Djekoun, J. M. Grenèche

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B2-structured FeAl was synthesized by an abrupt reaction during mechanical alloying (MA) of the elemental powders of Fe, Al and Ni. The structural, microstructural and morphological changes occurring in the studied material during MA were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Two crystalline phases were found, the major one corresponding to FeAl bcc phase with a crystallite size less than 10 nm, a lattice strain up to 1.6% and a dislocation density of about 2.3 1016m-2. The other phase in low proportion was corresponding to Fe (Al,Ni) solid solution. SEM images showed an irregular morphology of powder particles.

Keywords: mechanical alloying, ternary composition, dislocation density, structural properties

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Authors: Deb Kumar Shah, M. Shaheer Akhtar, Ha Ryeon Lee, O-Bong Yang, Chong Yeal Kim

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The crystalline silicon (Si) solar cells are highly renowned photovoltaic technology and well-established as the commercial solar technology. Most of the solar panels are globally installed with the crystalline Si solar modules. At the present scenario, the major photovoltaic (PV) market is shared by c-Si solar cells, but the cost of c-Si panels are still very high as compared with the other PV technology. In order to reduce the cost of Si solar panels, few necessary steps such as low-cost Si manufacturing, cheap antireflection coating materials, inexpensive solar panel manufacturing are to be considered. It is known that the antireflection (AR) layer in c-Si solar cell is an important component to reduce Fresnel reflection for improving the overall conversion efficiency. Generally, Si wafer exhibits the 30% reflection because it normally poses the two major intrinsic drawbacks such as; the spectral mismatch loss and the high Fresnel reflection loss due to the high contrast of refractive indices between air and silicon wafer. In recent years, researchers and scientists are highly devoted to a lot of researches in the field of searching effective and low-cost AR materials. Silicon nitride (SiNx) is well-known AR materials in commercial c-Si solar cells due to its good deposition and interaction with passivated Si surfaces. However, the deposition of SiNx AR is usually performed by expensive plasma enhanced chemical vapor deposition (PECVD) process which could have several demerits like difficult handling and damaging the Si substrate by plasma when secondary electrons collide with the wafer surface for AR coating. It is very important to explore new, low cost and effective AR deposition process to cut the manufacturing cost of c-Si solar cells. One can also be realized that a nano-texturing process like the growth of nanowires, nanorods, nanopyramids, nanopillars, etc. on Si wafer can provide a low reflection on the surface of Si wafer based solar cells. The above nanostructures might be enhanced the antireflection property which provides the larger surface area and effective light trapping. In this work, we report on the development of crystalline Si solar cells without using the AR layer. The Silicon wafer was modified by growing nanowires like Si nanostructures using the wet controlled etching method and directly used for the fabrication of Si solar cell without AR. The nanostructures over Si wafer were optimized in terms of sizes, lengths, and densities by changing the etching conditions. Well-defined and aligned wires like structures were achieved when the etching time is 20 to 30 min. The prepared Si nanostructured displayed the minimum reflectance ~1.64% at 850 nm with the average reflectance of ~2.25% in the wavelength range from 400-1000 nm. The nanostructured Si wafer based solar cells achieved the comparable power conversion efficiency in comparison with c-Si solar cells with SiNx AR layer. From this study, it is confirmed that the reported method (controlled wet etching) is an easy, facile method for preparation of nanostructured like wires on Si wafer with low reflectance in the whole visible region, which has greater prospects in developing c-Si solar cells without AR layer at low cost.

Keywords: chemical etching, conversion efficiency, silicon nanostructures, silicon solar cells, surface modification

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Authors: Shalini Arora, Sri Sivakumar

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The deep removal of high molecular weight sulphur compounds (e.g., 4,6, dimethyl dibenzothiophene) is challenging due to their steric hindrance. Hydrogenation desulfurization (HYD) pathway is the main pathway to remove these sulfur compounds, and it is mainly governed by the number of type 2 sites. The formation of type 2 sites can be enhanced by modulating the pore structure and the interaction between the active metal and support. To this end, we report the enhanced HDS catalytic activity of ultrasmall NiMo supported on amorphous alumina (A-Al₂O₃) catalysts by one pot colloidal synthesis method followed by calcination and sulfidation. The amorphous alumina (A-Al₂O₃) was chosen as the support due to its lower surface energy, better physicochemical properties, and enhanced acidic sites (due to the dominance of tetra and penta coordinated [Al] sites) than crystalline alumina phase. At 20% metal oxide composition, NiMo supported on A-Al₂O₃ catalyst showed 1.4 and 1.2 times more reaction rate constant and turn over frequency (TOF) respectively than the conventional catalyst (wet impregnated NiMo catalysts) for HDS reaction of dibenzothiophene reactant molecule. A-Al₂O₃ supported catalysts represented enhanced type 2 sites formation (because this catalystpossesses higher sulfidation degree (80%) and NiMoS sites (19.3 x 10¹⁷ sites/mg) with desired optimum stacking degree (2.5) than wet impregnated catalyst at same metal oxide composition 20%) along with higher active metal dispersion, Mo edge site fraction. The experimental observations were also supported by DFT simulations. Lower heat of adsorption (< 4.2 ev for MoS2 interaction and < 3.15 ev for Ni doped MoS2 interaction) values for A-Al₂O₃ confirmed the presence of weaker metal-support interaction in A-Al₂O₃ in contrast to crystalline ℽ-Al₂O3. The weak metal-support interaction for prepared catalysts clearly suggests the higher formation of type 2 sites which leads to higher catalytic activity for HDS reaction.

Keywords: amorphous alumina, colloidal, desulfurization, metal-support interaction

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Authors: F. Sevim, E. Sevimli, F. Demir, T. Çalban

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For the first time, nanofibers of PVA /nickel nitrate/silica/alumina izopropoxide/boric acid composite were prepared by using sol-gel processing and electrospinning technique. By high temperature calcinations of the above precursor fibers, nanofibers of NiO/Al2O3/B2O3/SiO2 composite with diameters of 500 nm could be successfully obtained. The fibers were characterized by TG/DTA, FT-IR, XRD and SEM analyses.

Keywords: nano fibers, NiO/Al2O3/B2O3/SiO2 composite, sol-gel processing, electro spinning

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Authors: Yi Hu, Chun-Chi Lin, Shau-En Yeh, Shin Lee

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In this study, p–n heterojunctions with La0.5Sr0.5CoO3 (LSCO) and W-doped VO2 thin films were fabricated by the radio frequency (r.f.) magnetron sputtering technique and sol-gel process, respectively. The thickness of VO2 and LSCO thin films are about 40 nm and 400 nm, respectively. Good crystalline match between LSCO and VO2 films was observed from the SEM. The built-in voltages for the junction are about 1.1 V and 2.3 V for the sample in the metallic and insulating state, respectively. The sample can undergo the current induced MIT during applying field when the sample was heated at 40 and 50ºC. This is in agreement with the value obtained from the difference in the work functions of LSCO and VO2. The band structure of the heterojunction was proposed based on the results of analysis.

Keywords: hetrojection, Mott transition, switching , VO2

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Authors: Sh. Sohrabnezhad, A. Jafarzadeh

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In this paper, MCM-41 mesoporous material nanofibers were synthesized by an electrospinning technique. The nanofibers were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), x-ray diffraction (XRD), and nitrogen adsorption–desorption measurement. Tetraethyl orthosilicate (TEOS) and polyvinyl alcohol (PVA) were used as a silica source and fiber forming source, respectively. TEM and SEM images showed synthesis of MCM-41 nanofibers with a diameter of 200 nm. The pore diameter and surface area of calcined MCM-41 nanofibers was 2.2 nm and 970 m²/g, respectively. The morphology of the MCM-41 nanofibers depended on spinning voltages.

Keywords: electrospinning, electron microscopy, fiber technology, porous materials, X-ray techniques

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Authors: Luís F. da Silva, Ariadne C. Catto, Osmando F. Lopes, Khalifa Aguir, Valmor R. Mastelaro, Caue Ribeiro, Elson Longo

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Gas detection is important for controlling industrial, and vehicle emissions, agricultural residues, and environmental control. In last decades, several semiconducting oxides have been used to detect dangerous or toxic gases. The excellent gas-sensing performance of these devices have been observed at high temperatures (~250 °C), which forbids the use for the detection of flammable and explosive gases. In this way, ultraviolet light activated gas sensors have been a simple and promising alternative to achieve room temperature sensitivity. Among the semiconductor oxides which exhibit a good performance as gas sensor, the zinc oxide (ZnO) and tin oxide (SnO2) have been highlighted. Nevertheless, their poor selectivity is the main disadvantage for application as gas sensor devices. Recently, heterostructures combining these two semiconductors (ZnO-SnO2) have been studied as an alternative way to enhance the gas sensor performance (sensitivity, selectivity, and stability). In this work, we investigated the influence of mass ratio Zn:Sn on the properties of ZnO-SnO2 nanocomposites prepared by hydrothermal treatment for 4 hours at 200 °C. The crystalline phase, surface, and morphological features were characterized by X-ray diffraction (XRD), high-resolution transmission electron (HR-TEM), and X-ray photoelectron spectroscopy (XPS) measurements. The gas sensor measurements were carried out at room-temperature under ultraviolet (UV) light irradiation using different ozone levels (0.06 to 0.61 ppm). The XRD measurements indicate the presence of ZnO and SnO2 crystalline phases, without the evidence of solid solution formation. HR-TEM analysis revealed that a good contact between the SnO2 nanoparticles and the ZnO nanorods, which are very important since interface characteristics between nanostructures are considered as challenge to development new and efficient heterostructures. Electrical measurements proved that the best ozone gas-sensing performance is obtained for ZnO:SnO2 (50:50) nanocomposite under UV light irradiation. Its sensitivity was around 6 times higher when compared to SnO2 pure, a traditional ozone gas sensor. These results demonstrate the potential of ZnO-SnO2 heterojunctions for the detection of ozone gas at room-temperature when irradiated with UV light irradiation.

Keywords: hydrothermal, zno-sno2, ozone sensor, uv-activation, room-temperature

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Authors: Nastaran Hazrati, Ali Akbar Miran Beigi, Majid Abdouss, Amir Vahid

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Hydrogen sulfide is the most toxic gas of crude oil. Adsorption is an energy-efficient process used to remove undesirable compounds such as H2S in gas or liquid streams by passing the stream through a media bed composed of an adsorbent. In this study, H2S of Iran crude oil was separated via cold stripping then zinc incorporated MCM-41 was synthesized via an in-situ method. ZnO functionalized mesoporous silica samples were characterized by XRD, N2 adsorption and TEM. The obtained results of adsorption of H2S showed superior ability of all the materials and with an increase in ZnO amount adsorption was increased.

Keywords: MCM-41, ZnO, H2S removal, adsorption

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Authors: Aniruddha Mitra, Abbas Rashidi, Shane Lewis, Jefferson Doehling, Alexis Pawlak, Jacob Schwartz, Imaobong Ekpo, Atin Adhikari

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Working or living close to demolition sites can increase risks of dust-related health problems. Demolition of concrete buildings may produce crystalline silica dust, which can be associated with a broad range of respiratory diseases including silicosis and lung cancers. Previous studies demonstrated significant associations between demolition dust exposure and increase in the incidence of mesothelioma or asbestos cancer. Dust is a generic term used for minute solid particles of typically <500 µm in diameter. Dust particles in demolition sites vary in a wide range of sizes. Larger particles tend to settle down from the air. On the other hand, the smaller and lighter solid particles remain dispersed in the air for a long period and pose sustained exposure risks. Submicron ultrafine particles and nanoparticles are respirable deeper into our alveoli beyond our body’s natural respiratory cleaning mechanisms such as cilia and mucous membranes and are likely to be retained in the lower airways. To our knowledge, how various demolition tasks release nanoparticles are largely unknown and previous studies mostly focused on course dust, PM2.5, and PM10. General belief is that the dust generated during demolition tasks are mostly large particles formed through crushing, grinding, or sawing of various concrete and wooden structures. Therefore, little consideration has been given to the generated submicron ultrafine and nanoparticles and their exposure levels. These data are, however, critically important because recent laboratory studies have demonstrated cytotoxicity of nanoparticles on lung epithelial cells. The above-described knowledge gaps were addressed in this study by a novel newly developed nanoparticle monitor, which was used for nanoparticle monitoring at two adjacent indoor and outdoor building demolition sites in southern Georgia. Nanoparticle levels were measured (n = 10) by TSI NanoScan SMPS Model 3910 at four different distances (5, 10, 15, and 30 m) from the work location as well as in control sites. Temperature and relative humidity levels were recorded. Indoor demolition works included acetylene torch, masonry drilling, ceiling panel removal, and other miscellaneous tasks. Whereas, outdoor demolition works included acetylene torch and skid-steer loader use to remove a HVAC system. Concentration ranges of nanoparticles of 13 particle sizes at the indoor demolition site were: 11.5 nm: 63 – 1054/cm³; 15.4 nm: 170 – 1690/cm³; 20.5 nm: 321 – 730/cm³; 27.4 nm: 740 – 3255/cm³; 36.5 nm: 1,220 – 17,828/cm³; 48.7 nm: 1,993 – 40,465/cm³; 64.9 nm: 2,848 – 58,910/cm³; 86.6 nm: 3,722 – 62,040/cm³; 115.5 nm: 3,732 – 46,786/cm³; 154 nm: 3,022 – 21,506/cm³; 205.4 nm: 12 – 15,482/cm³; 273.8 nm: Keywords: demolition dust, industrial hygiene, aerosol, occupational exposure

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Authors: M. Bischoff, F. Schmidt, J. Herrmann, J. Mattheß, G. Seide, T. Gries

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Crop yields have not increased as dramatically as the demand for food. One method to counteract this is to use pesticides to keep away predators, e.g. several forms of insecticide are available to fight insects. These insecticides and pesticides are both controversial as their application and their residue in the food product can also harm humans. In this study an alternative method to combat insects is studied. A physical insect-killing effect of SiO₂ particles is used. The particles are applied on fibres to avoid erosion in the fields, which would occur when applied separately. The development of such SiO₂ functionalized PP fibres is shown.

Keywords: agriculture, environment, insects, protection, silica, textile

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Authors: Przemyslaw Brzyski, Stanislaw Fic

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Hydrated lime, because of the life cycle (return to its natural form as a result of the setting and hardening) has a positive environmental impact. The lime binder is used in mortars. Lime is a slow setting binder with low mechanical properties. The aim of the study was to evaluate the possibility of improving the properties of the lime binder by using different pozzolanic materials as partial replacement of hydrated lime binder. Pozzolan materials are the natural or industrial waste, so do not affect the environmental impact of the lime binder. The following laboratory tests were performed: the analysis of the physical characteristics of the tested samples of lime mortars (bulk density, porosity), flexural and compressive strength, water absorption and the capillary rise of samples and consistency of fresh mortars. As a partial replacement of hydrated lime (in the amount of 10%, 20%, 30% by weight of lime) a metakaolin, silica fume, and zeolite were used. The shortest setting and hardening time showed mortars with the addition of metakaolin. All additives noticeably improved strength characteristic of lime mortars. With the increase in the amount of additive, the increase in strength was also observed. The highest flexural strength was obtained by using the addition of metakaolin in an amount of 20% by weight of lime (2.08 MPa). The highest compressive strength was obtained by using also the addition of metakaolin but in an amount of 30% by weight of lime (9.43 MPa). The addition of pozzolan caused an increase in the mortar tightness which contributed to the limitation of absorbability. Due to the different surface area, pozzolanic additives affected the consistency of fresh mortars. Initial consistency was assumed as plastic. Only the addition of silica fume an amount of 20 and 30% by weight of lime changed the consistency to the thick-plastic. The conducted study demonstrated the possibility of applying lime mortar with satisfactory properties. The features of lime mortars do not differ significantly from cement-based mortar properties and show a lower environmental impact due to CO₂ absorption during lime hardening. Taking into consideration the setting time, strength and consistency, the best results can be obtained with metakaolin addition to the lime mortar.

Keywords: lime, binder, mortar, pozzolan, properties

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Authors: Amanda C. Q. M. Vieira, Cybelly M. Melo, Camila B. M. Figueirêdo, Giovanna C. R. M. Schver, Salvana P. M. Costa, Magaly A. M. de Lyra, Ping I. Lee, José L. Soares-Sobrinho, Pedro J. Rolim-Neto, Mônica F. R. Soares

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Epiisopiloturine (EPI) is a drug candidate that is extracted from Pilocarpus microphyllus and isolated from the waste of Pilocarpine. EPI has demonstrated promising schistosomicidal, leishmanicide, anti-inflammatory and antinociceptive activities, according to in vitro studies that have been carried out since 2009. However, this molecule shows poor aqueous solubility, which represents a problem for the release of the drug candidate and its absorption by the organism. The purpose of the present study is to investigate the extent of enhancement of kinetic solubility of a solid solution (SS) of EPI in hipromellose phthalate HP-55 (HPMCP), an enteric polymer carrier. SS was obtained by the solvent evaporation methodology, using acetone/methanol (60:40) as solvent system. Both EPI and polymer (drug loading 10%) were dissolved in this solvent until a clear solution was obtained, and then dried in oven at 60ºC during 12 hours, followed by drying in a vacuum oven for 4 h. The results show a considerable modification in the crystalline structure of the drug candidate. For instance, X-ray diffraction (XRD) shows a crystalline behavior for the EPI, which becomes amorphous for the SS. Polarized light microscopy, a more sensitive technique than XRD, also shows completely absence of crystals in SS sample. Differential Scanning Calorimetric (DSC) curves show no signal of EPI melting point in SS curve, indicating, once more, no presence of crystal in this system. Interaction between the drug candidate and the polymer were found in Infrared microscopy, which shows a carbonyl 43.3 cm-1 band shift, indicating a moderate-strong interaction between them, probably one of the reasons to the SS formation. Under sink conditions (pH 6.8), EPI SS had its dissolution performance increased in 2.8 times when compared with the isolated drug candidate. EPI SS sample provided a release of more than 95% of the drug candidate in 15 min, whereas only 45% of EPI (alone) could be dissolved in 15 min and 70% in 90 min. Thus, HPMCP demonstrates to have a good potential to enhance the kinetic solubility profile of EPI. Future studies to evaluate the stability of SS are required to conclude the benefits of this system.

Keywords: epiisopiloturine, hipromellose phthalate HP-55, pharmaceuticaltechnology, solubility

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Authors: Laura Vitola, Diana Bajare, Genadijs Sahmenko, Girts Bumanis

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About 8 % of CO2 emission in the world is produced by concrete industry therefore replacement of cement in concrete composition by additives with pozzolanic activity would give a significant impact on the environment. Material which contains silica SiO2 or amorphous silica SiO2 together with aluminum dioxide Al2O3 is called pozzolana type additives in the concrete industry. Pozzolana additives are possible to obtain from recycling industry and different production by-products such as processed bulb boric silicate (DRL type) and lead (LB type) glass, coal combustion bottom ash, utilized brick pieces and biomass ash, thus solving utilization problem which is so important in the world, as well as practically using materials which previously were considered as unusable. In the literature, there is no summarized method which could be used for quick waste-product pozzolana activity evaluation without the performance of wide researches related to the production of innumerable concrete contents and samples in the literature. Besides it is important to understand which parameters should be predicted to characterize the efficiency of waste-products. Simple methods of pozzolana activity increase for different types of waste-products are also determined. The aim of this study is to evaluate effectiveness of the different types of waste materials and industrial by-products (coal combustion bottom ash, biomass ash, waste glass, waste kaolin and calcined illite clays), and determine which parameters have the greatest impact on pozzolanic activity. By using materials, which previously were considered as unusable and landfilled, in concrete industry basic utilization problems will be partially solved. The optimal methods for treatment of waste materials and industrial by–products were detected with the purpose to increase their pozzolanic activity and produce substitutes for cement in the concrete industry. Usage of mentioned pozzolanic allows us to replace of necessary cement amount till 20% without reducing the compressive strength of concrete.

Keywords: cement substitutes, micro and nano fillers, pozzolanic properties, specific surface area, particle size, waste products

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Authors: Damien Rinsant, Eugen Andreiadis, Michael Carboni, Daniel Meyer

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Different types of materials have been developed for the solid/liquid uranium extraction processes, such as functionalized organic polymers, hybrid silica or inorganic adsorbents. In general, these materials exhibit a moderate affinity for uranyl ions and poor selectivity against impurities like iron, vanadium or molybdenum. Moreover, the structural organization deficiency of these materials generates ion diffusion issues inside the material. Therefore, the aim of our study is to developed efficient and organized materials, stable in the acid media encountered in uranium extraction processes. Metal organic frameworks (MOFs) are hybrid crystalline materials consisting of an inorganic part (cluster or metal ions) and tailored organic linkers connected via coordination bonds. These hierarchical materials have exceptional surface area, thermal stability and a large variety of tunable structures. However, due to the reversibility of constitutive coordination bonds, MOFs have moderate stability in strongly complexing or acidic media. Only few of them are known to be stable in aqueous media and only one example is described in strong acidic media. However, these conditions are very often encountered in the environmental pollution remediation of mine wastewaters. To tackle the challenge of developing MOFs adapted for uranium extraction from acid mine waters, we have investigated the stability of several materials. To ensure a good stability we have synthetized and characterized different materials based on highly coordinated metal clusters, such as LnOFs and Zirconium based materials. Among the latter, the UiO family shows a great stability in sulfuric acid media even in the presence of 1.4 M sodium sulfate at pH 2. However, the stability in phosphoric media is reduced due to the high affinity between zirconium and phosphate ligand. Based on these results, we have developed a tertiary amine functionalized MOF denoted UiO-68-NMe2 particularly adapted for the extraction of anionic uranyl (VI) sulfate complexes mainly present in the acid mine solutions. The adsorption capacity of the material has been determined upon varying total sulfate concentration, contact time and uranium concentration. The extraction tests put in evidence different phenomena due to the complexity of the extraction media and the interaction between the MOF and sulfate anion. Finally, the extraction mechanisms and the interaction between uranyl and the MOF structure have been investigated. The functionalized material UiO-68-NMe2 has been characterized in the presence and absence of uranium by FT-IR, UV and Raman techniques. Moreover, the stability of the protonated amino functionalized MOF has been evaluated. The synthesis, characterization and evaluation of this type of hybrid material, particularly adapted for uranium extraction in sulfuric acid media by an anionic exchange mechanism, paved the way for the development of metal organic frameworks functionalized by different other chelating motifs, such as bifunctional ligands showing an enhanced affinity and selectivity for uranium in acid and complexing media. Work in this direction is currently in progress.

Keywords: extraction, MOF, ligand, uranium

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Authors: H. Assaedi, F. U. A. Shaikh, I. M. Low

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This paper presents the effects of mixing procedures on mechanical properties of flyash-based geopolymer matrices containing nanosilica (NS) at 0.5%, 1.0%, 2.0%, and 3.0% by wt.. Comparison is made with conventional mechanical dry-mixing of NS with flyash and wet-mixing of NS in alkaline solutions. Physical and mechanical properties are investigated using X-Ray Diffraction (XRD) and Scanning Electron Microscope (SEM). Results show that generally the addition of NS particles enhanced the microstructure and improved flexural and compressive strengths of geopolymer nanocomposites. However, samples prepared using dry-mixing approach demonstrate better physical and mechanical properties than wet-mixing of NS.

Keywords: geopolymer, nano-silica, dry mixing, wet mixing, physical properties, mechanical properties

Procedia PDF Downloads 245