Search results for: Dispersive liquid-liquid microextraction

Authors: Kishor C. Poria, Deepak Adroja, Arvind Bajaj

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During the last few decades, the growth of single crystals has attained enormous importance for both academic research and technology. Single crystals are pillars of modern technology. In recent emerging trends of photonics and optoelectronics technology, there has been increased need for organic and semi organic materials for Non-Linear Optical (NLO) applications. The paper dealt with the initiation of good single crystals of thiourea and metal doped thiourea. The authors have successfully grown thiourea (pure) and metal doped thiourea crystals using relatively simple and inexpensive slow evaporation of aqueous solution technique. Pure thiourea crystals were grown with different light intensities and frequencies as there growth conditions. Metals (Cu, Co, Ni, Fe) doped crystals were grown using a simple evaporation technique. The paper explains growth methods and associated grown parameters in detail. The average size of the crystal is varied in size from 40 mm x 1mm to 1.5 mm x 1.5 mm to 0.5 mm. Crystals obtained are hexagonal, tetragonal, and rectangular in shape with different optical qualities. All grown crystals are characterized using X-Ray Diffraction Analysis (XRD), Ultra Violet Visible analysis, and Fourier Transform Infrared Spectrometry. Their non-linear optical characteristics were determined by Second Harmonic Generation (SHG) and their Laser Dispersive analysis. The grown crystals are characterized using Nd:YAG laser and the highest conversion efficiency of the signal pass light are calculated. It shows 58 % of standard values for KDP crystals. All results are summarized in this work.

Keywords: crystal, metal-doped thiourea, non-linear optical, NLO, thiourea

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Authors: Monika Šípová, Daniela Marušáková, Claudia Aparicio

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New sources and ways of producing energy are still seeking, and one of the sustainable ways is Generation IV nuclear reactors. The supercritical water-cooled reactor is one of the six nuclear reactors of Generation IV, and as a consequence of the development of light water, reactors seem to be the most perspective. Thus, materials usually used in light water reactors are also tested under the expected operating conditions of the supercritical water-cooled reactor. Austenitic stainless steel 08Cr18Ni10Ti is widely used in the eastern types of light water nuclear power plants. Therefore, specimens of 08Cr18Ni10Ti were exposed to conditions close to the pseudo-critical point of water and high-temperature supercritical water. The description and evaluation of the corrosion behaviour of austenitic stainless steel have been done based on the results of X-ray diffraction in combination with energy dispersive spectroscopy and electron backscatter diffraction. Thus, significant differences have been found in the structure and composition of oxides formed depending on the temperature of exposure. The high temperature of supercritical water resulted in localised form of corrosion in contrast to the thin oxide layer of 1 µm present on the surface of specimens exposed close to the pseudo-critical point of water. The obtained results are important for further research as the supercritical water can be successfully used as a coolant for small modular reactors, which are currently of interest.

Keywords: localised corrosion, supercritical water, stainless steel, electron backscatter diffraction

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Authors: Yi-Chun Wu, Nai-Yun Chang, Chuan LI

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This study investigates a feasible range of composition for the mixture of gelatin and polyvinyl alcohol to form nanofibers by electrospinning. Gelatin, one of the most available naturally derived hydrogels of amino acids, is a popular choice for food additives, cosmetic ingredients, biomedical implants, or dressing of its non-toxic and biodegradable nature. Nevertheless, synthetic hydrogel polyvinyl alcohol has long been used as a thickening agent for adhesion purposes. Many biomedical devices are also containing polyvinyl-alcohol as a major content, such as eye drops and contact lenses. To discover appropriate compositions of gelatin and polyvinyl-alcohol for electrospun nanofibers, polymer solutions of different volumetric ratios between gelatin and polyvinyl alcohol were prepared for electrospinning. The viscosity, surface tension, pH value, and electrical conductance of polymer solutions were measured. On the nanofibers, the vibrational modes of molecular structures in nanofibers were investigated by Fourier-transform infrared spectroscopy. The morphologies and surface chemical elements of fibers were examined by the scanning electron microscope and the energy-dispersive X-ray spectroscopy. The hydrophilicity of nanofiberswas evaluated by the water contact angles on the surface of the fibers. To further test the biotoxicity of nanofibers, an in-vitro 3T3 fibroblasts culture further tested the biotoxicity of the electrospun nanofibers. Throughstatistical analyses of the experimental data, it is found that the polyvinyl-alcohol rich composition (the volumetric ratio of gelatin/polyvinyl-alcohol < 1) would be a preferable choice for the formation of nanofibers by the current setup of electrospinning. These electrospun nanofibers tend to be hydrophilic with no biotoxicity threat to the 3T3 fibroblasts.

Keywords: gelatin, polyvinyl-alcohol, nanofibers, electrospinning, spin coating

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Authors: Rejane Maria P. da Silva, Mariana X. Milagre, João Victor de S. Araujo, Leandro A. de Oliveira, Renato A. Antunes, Isolda Costa

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The Al-Cu-Li alloys are advanced materials for aerospace application because of their interesting mechanical properties and low density when compared with conventional Al-alloys. However, Al-Cu-Li alloys are susceptible to localized corrosion. The near-surface deformed layer (NSDL) induced by the rolling process during the production of the alloy and its removal by polishing can influence on the corrosion susceptibility of these alloys. In this work, the influence of surface preparation effects on the electrochemical activity of AA2098-T351 (Al–Cu–Li alloy) was investigated using a correlation between surface chemistry, microstructure, and electrochemical activity. Two conditions were investigated, polished and as-received surfaces of the alloy. The morphology of the two types of surfaces was investigated using confocal laser scanning microscopy (CLSM) and optical microscopy. The surface chemistry was analyzed by X-ray Photoelectron Spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDS). Global electrochemical techniques (potentiodynamic polarization and EIS technique) and a local electrochemical technique (Localized Electrochemical Impedance Spectroscopy-LEIS) were used to examine the electrochemical activity of the surfaces. The results obtained in this study showed that in the as-received surface, the near-surface deformed layer (NSDL), which is composed of Mg-rich bands, influenced the electrochemical behavior of the alloy. The results showed higher electrochemical activity to the polished surface condition compared to the as-received one.

Keywords: Al-Cu-Li alloys, surface preparation effects, electrochemical techniques, localized corrosion

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Authors: Sara Mercedes Barroso Pinzón, Antonio Javier Sanchéz Herencia, Begoña Ferrari, Álvaro Jesús Castro

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The current need for durable implants and bone substitutes characterised by biocompatibility, bioactivity and mechanical properties, without immunological rejection, is a major challenge for scientists. Hydroxyapatite (HAp) has been considered for decades as an ideal biomaterial for bone regeneration due to its chemical and crystallographic similarity to the mineral structure bioapatites. However, the lack of trace elements in the hydroxyapatite structure gives it very low mechanical and biological properties. In this sense, the objective of the research is to address the synthesis of hydroxyapatite with Mg from phosphate rock from sedimentary deposits in the central-eastern region of Colombia, taking advantage of the release of the species contained as natural precursors of Ca, P and Mg. The minerals present were studied, fluorapatite as the mineral of interest associated with mineralogical species of magnesium carbonates and quartz. The chemical and mineralogical composition was determined by X-ray fluorescence (XRF) and X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX); as well as the evaluation of the surface physicochemical properties of zeta potential (PZC), with the aim of studying the surface behaviour of the microconstituents present in the phosphate rock and to elucidate the synergistic mechanism between the minerals and establish the optimum conditions for the wet concentration process. From the products obtained and characterised by XRD, XRF, SEM, FTIR, RAMAN, HAp-Mg biocomposite scaffolds are fabricated and the influence of Mg on the morphometric parameters, mechanical and biological properties of the designed materials is evaluated.

Keywords: phosphate rock, hydroxyapatite, magnesium, biomaterials

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Authors: Wilson Handoko, Farshid Pahlevani, Isha Singla, Himanish Kumar, Veena Sahajwalla

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Aluminium bronze alloys are well known for their superior abrasion, tensile strength and non-magnetic properties, due to the co-presence of iron (Fe) and aluminium (Al) as alloying elements and have been commonly used in many industrial applications. However, continuous exposure to the marine environment will accelerate the risk of a tendency to Al bronze alloys parts failures. Although a higher level of corrosion resistance properties can be achieved by modifying its elemental composition, it will come at a price through the complex manufacturing process and increases the risk of reducing the ductility of Al bronze alloy. In this research, the use of ironmaking slag and waste plastic as the input source for surface modification of Al bronze alloy was implemented. Microstructural analysis conducted using polarised light microscopy and scanning electron microscopy (SEM) that is equipped with energy dispersive spectroscopy (EDS). An electrochemical corrosion test was carried out through Tafel polarisation method and calculation of protection efficiency against the base-material was determined. Results have indicated that uniform modified surface which is as the result of selective diffusion process, has enhanced corrosion resistance properties up to 12.67%. This approach has opened a new opportunity to access various industrial utilisations in commercial scale through minimising the dependency on natural resources by transforming waste sources into the protective coating in environmentally friendly and cost-effective ways.

Keywords: aluminium bronze, waste-based surface modification, tafel polarisation, corrosion resistance

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Authors: Jason Ting Jing Cheng, Lee Foo Wei, Yew Ming Kun, Chin Ren Jie, Yip Chun Chieh

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The utilization of industrial by-products, such as steel slag in cementitious materials, not only mitigates environmental impact but also enhances material properties. This study investigates the dual influence of steel slag particle size on the compressive strength and carbonation efficiency of cementitious composites. Through a systematic experimental approach, steel slag particles were incorporated into cement at varying sizes, and the resulting composites were subjected to mechanical and carbonation tests. Scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) are conducted in this paper. The findings reveal a positive correlation between increased particle size and compressive strength, attributed to the improved interfacial transition zone and packing density. Conversely, smaller particle sizes exhibited enhanced carbonation efficiency, likely due to the increased surface area facilitating the carbonation reaction. The presence of higher silica and calcium content in finer particles was confirmed by EDX, which contributed to the accelerated carbonation process. This study underscores the importance of particle size optimization in designing sustainable cementitious materials with balanced mechanical performance and carbon sequestration potential. The insights gained from the advanced analytical techniques offer a comprehensive understanding of the mechanisms at play, paving the way for the strategic use of steel slag in eco-friendly construction practices.

Keywords: steel slag, carbonation efficiency, particle size enhancement, compressive strength

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Authors: Fares Khalfallah, Zakaria Boumerzoug, Selvarajan Rajakumar, Elhadj Raouache

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The ceramic-aluminum bond is strongly present in industrial tools, due to the need to combine the properties of metals, such as ductility, thermal and electrical conductivity, with ceramic properties like high hardness, corrosion and wear resistance. In recent years, some joining techniques have been developed to achieve a good bonding between these materials such as brazing, diffusion bonding, ultrasonic joining and friction welding. In this work, AA1100 aluminum alloy rods were welded with Alumina 99.9 wt% ceramic rods, by friction welding. The effect of friction pressure on mechanical and structural properties of welded joints was studied. The welding was performed by direct friction welding machine. The welding samples were rotated at a constant rotational speed of 900 rpm, friction time of 4 sec, forging strength of 18 MPa, and forging time of 3 sec. Three different friction pressures were applied to 20, 34 and 45 MPa. The three-point bending test and Vickers microhardness measurements were used to evaluate the strength of the joints and investigate the mechanical properties of the welding area. The microstructure of joints was examined by optical microscopy (OM), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The results show that bending strength increased, and then decreased after reaching a maximum value, with increasing friction pressure. The SEM observation shows that the increase in friction pressure led to the appearance of cracks in the microstructure of the interface area, which is decreasing the bending strength of joints.

Keywords: welding of ceramic to aluminum, friction welding, alumina, AA1100 aluminum alloy

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Authors: Shimaa A. Higazy, Olfat E. El-Azabawy, Ahmed M. Al-Sabagh, Notaila M. Nasser, Eman A. Khamis

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In this work, two novel Schiff base polymers (PSB1 and PSB₂) with extra-high protective barrier features were facilely prepared via Polycondensation reactions. They were applied for the first time as effective corrosion inhibitors in the sour corrosive media of petroleum environments containing hydrogen sulfide (H₂S) gas. For studying the polymers' inhibitive action on the carbon steel, numerous corrosion testing methods including potentiodynamic polarization (PDP), open circuit potential, and electrochemical impedance spectroscopy (EIS) have been employed at various temperatures (298-328 K) in the oil wells formation water with H₂S concentrations of 100, 400, and 700 ppm as aggressive media. The activation energy (Ea) and other thermodynamic parameters were computed to describe the mechanism of adsorption. The corrosion morphological traits and steel samples' surfaces composition were analyzed by field emission scanning electron microscope and energy dispersive X-ray analysis. The PSB2 inhibited sour corrosion more effectively than PSB1 when subjected to electrochemical testing. The 100 ppm concentration of PSB2 exhibited 82.18 % and 81.14 % inhibition efficiencies at 298 K in PDP and EIS measurements, respectively. While at 328 K, the inhibition efficiencies were 61.85 % and 67.4 % at the same dosage and measurements. These poly Schiff bases exhibited fascinating performance as corrosion inhibitors in sour environment. They provide a great corrosion inhibition platform for the sustainable future environment.

Keywords: schiff base polymers, corrosion inhibitors, sour corrosive media, potentiodynamic polarization, H₂S concentrations

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Authors: Bright Kwakye-Awuah, Elizabeth Von-Kiti, Isaac Nkrumah, Baah Sefa-Ntiri, Craig D. Williams

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Bauxite and kaolin from Ghana Bauxite Company mine site were used to synthesize zeolites. Bauxite served as the alumina source and kaolin the silica source. Synthesis variations include variation of aging time at constant crystallization time and variation of crystallization times at constant aging time. Characterization techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive x-ray analysis (EDX) and Fourier transform infrared spectroscopy (FTIR) were employed in the characterization of the raw samples as well as the synthesized samples. The results obtained showed that the transformations that occurred and the phase of the resulting products were coordinated by the aging time, crystallization time, alkaline concentration and Si/Al ratio of the system. Zeolites A, X, Y, analcime, Sodalite, and ZK-14 were some of the phases achieved. Zeolite LTA was achieved with short crystallization times of 3, 5, 18 and 24 hours and a maximum aging of 24 hours. Zeolite LSX was synthesized with 24 hr aging followed with 24 hr hydrothermal treatment whilst zeolite Y crystallized after 48 hr of aging and 24 hr crystallization. Prolonged crystallization time produced a mixed phased product. Prolonged aging times, on the other hand, did not yield any zeolite as the sample was amorphous. Increasing the alkaline content of the reaction mixture above 5M introduced sodalite phase in the final product. The properties of the final products were comparable to zeolites synthesized from pure chemical reagents.

Keywords: bauxite, kaolin, aging, crystallization, zeolites

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Authors: Shefaa Mansour, Hassan Arafat, Shadi Hasan

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Management of reverse osmosis (RO) brine has become a major area of research due to the environmental concerns associated with it. This study worked on studying the feasibility of the direct contact membrane distillation (DCMD) system in the treatment of this RO brine. The system displayed great potential in terms of its flux and salt rejection, where different operating conditions such as the feed temperature, feed salinity, feed and permeate flow rates were varied. The highest flux of 16.7 LMH was reported with a salt rejection of 99.5%. Although the DCMD has displayed potential of enhanced water recovery from highly saline solutions, one of the major drawbacks associated with the operation is the fouling of the membranes which impairs the system performance. An operational run of 77 hours for the treatment of RO brine of 56,500 ppm salinity was performed in order to investigate the impact of fouling of the membrane on the overall operation of the system over long time operations. Over this time period, the flux was observed to have reduced by four times its initial flux. The fouled membrane was characterized through different techniques for the identification of the organic and inorganic foulants that have deposited on the membrane surface. The Infrared Spectroscopy method (IR) was used to identify the organic foulants where SEM images displayed the surface characteristics of the membrane. As for the inorganic foulants, they were identified using X-ray Diffraction (XRD), Ion Chromatography (IC) and Energy Dispersive Spectroscopy (EDS). The major foulants found on the surface of the membrane were inorganic salts such as sodium chloride and calcium sulfate.

Keywords: brine treatment, membrane distillation, fouling, characterization

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Authors: Nomthandazo Precious Sibiya, Thembisile Patience Mahlangu, Sudesh Rathilal

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Heavy metal removal is critical in the wastewater treatment process due to its numerous harmful effects on human and aquatic life. There are several chemical and physical techniques for removing heavy metals from wastewater, including ion exchange, reverse osmosis, adsorption, electrodialysis, and ultrafiltration. However, adsorption technology has captivated researchers for years due to its low cost, high efficiency, and compatible with the environment. In this study, the adsorption effectiveness of three modified agro-waste materials was explored for the removal of lead from synthetic wastewater: banana peels (BP), orange peels (OP), and sugarcane bagasse (SB). The magnetite (Fe₃O₄) is incorporated with BP, OP, and SB at a ratio of 1:1 to create magnetic biosorbents. Characterization of biosorbents was carried out using and scanning electron microscopy (SEM) combined with energy-dispersive X-ray (EDX) to investigate surface morphology and elemental compositions, respectively. A series of batch experiments were carried out to investigate the effects of adsorbent mass, agitation time, and initial pH concentration on adsorption behaviour, as well as adsorption isotherms and kinetics. The removal efficiency of lead by the modified agro-waste materials proved to be superior to that of non-modified agro-waste materials. The proof of concept was achieved, and agro-waste materials can be paired with adsorption technology to effectively remove lead from aqueous media. The use of agricultural waste as biosorbents will aid in waste reduction and management.

Keywords: adsorption, isotherms, kinetics, agro waste, nanoparticles, batch

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Authors: Daniel Ferreira, José M. Marques Oliveira, Filipe Oliveira

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Wear phenomena is critical in injection moulding processes, causing failure of the components, and making the parts more expensive with an additional wasting time. When very abrasive materials are being injected inside the steel mould’s cavities, such as polymers reinforced with abrasive fibres, the consequences of the wear are more evident. Maraging steel (1.2709) is commonly employed in moulding components to resist in very aggressive injection conditions. In this work, the wear performance of the SLM produced 1.2709 maraging steel reinforced by ultrafine titanium and tungsten carbide (TiC-WC), was investigated using a pin-on-disk testing apparatus. A polypropylene reinforced with 40 wt.% fibreglass (PP40) disk, was used as the counterpart material. The wear tests were performed at 40 N constant load and 0.4 ms-1 sliding speed at room temperature and humidity conditions. The experimental results demonstrated that the wear rate in the 18Ni300-TiC-WC composite is lower than the unreinforced 18Ni300 matrix. The morphology and chemical composition of the worn surfaces was observed by 3D optical profilometry and scanning electron microscopy (SEM), respectively. The resulting debris, caused by friction, were also analysed by SEM and energy dispersive X-ray spectroscopy (EDS). Their morphology showed distinct shapes and sizes, which indicated that the wear mechanisms, may be different in maraging steel produced by casting and SLM. The coefficient of friction (COF) was recorded during the tests, which helped to elucidate the wear mechanisms involved.

Keywords: selective laser melting, nanocomposites, injection moulding, polypropylene with fibreglass

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Authors: S. Nqayi, B. Sondezi

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A rare-earth-based Sm₂MnRuO₆₊δ (SMRO) double perovskite was prepared using a high-temperature solid-state reaction. The structural, morphological, chemical, thermodynamic, and magnetic properties were measured with X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), X-ray photoemission spectroscopy (XPS), and vibrating sample magnetometer (VSM), respectively. The XRD revealed a tetragonal structure belonging to the I4/mmm space group, number 139, with linear Mn−O−Ru bonds. Replacing the well-studied alkaline earth metal with a rare-earth element increased the Mn-O bond length difference between the shorter equatorial (Mn-Oab) and the axial (Mn-Oc) bonds by approximately 6.3%. The elemental composition showed an O-rich double perovskite with a Ru deficit, which encourages the formation of a Ru⁶⁺ (d²) state. XPS spectra of Sm-3d, Ru-3d, and Mn-2p revealed the coexistence of a double oxidation state for each cation; Sm²⁺, Sm³⁺, Ru³⁺, Ru⁶⁺, Mn²⁺ , and Mn³⁺, in varying proportions. Entropy studies showed drastic ordering of spins at low temperatures (up to 12.4 K), whilst increasing temperatures above this point resulted in a drastic increase of disorder of the spins (up to 43.26 K), beyond which a constant slope of entropy is observed. Magnetic measurements revealed two magnetic ground states at TN = 12.4 K and TC = 43.3 K ordering antiferromagnetically (AFM) and ferromagnetically (FM), respectively. Kneller fit further showed that the materials become completely paramagnetic at TB = 88.1 K, (the blocking temperature). The existence of ferromagnetic (FM) super-exchange coupling in this work originating from Mn³⁺ (t³₂𝓰e¹𝓰)−O−Ru³⁺ (t⁵₂𝓰e⁰𝓰) and Mn²⁺ (t³₂𝓰e²𝓰−O−Ru⁶⁺ (t²₂𝓰e⁰𝓰) which plays an important role in suppressing the Mn/Ru−O−Mn/Ru antiferromagnetic (AFM) interactions.

Keywords: solid-state reaction, super-exchange coupling, ferromagnetic, Kneller’s law, entropy

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Authors: Sze Shin Low, Michelle T. T. Tan, Poi Sim Khiew, Hwei-San Loh

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An efficient graphene/zinc oxide (PSE-G/ZnO) platform based on pi-pi stacking, non-covalent interactions for the development of aptamer-based biosensor was presented in this study. As a proof of concept, the DNA recognition capability of the as-developed PSE-G/ZnO enhanced aptamer-based biosensor was evaluated using Coconut Cadang-cadang viroid disease (CCCVd). The G/ZnO nanocomposite was synthesised via a simple, green and efficient approach. The pristine graphene was produced through a single step exfoliation of graphite in sonochemical alcohol-water treatment while the zinc nitrate hexahydrate was mixed with the graphene and subjected to low temperature hydrothermal growth. The developed facile, environmental friendly method provided safer synthesis procedure by eliminating the need of harsh reducing chemicals and high temperature. The as-prepared nanocomposite was characterised by X-ray diffractometry (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) to evaluate its crystallinity, morphology and purity. Electrochemical impedance spectroscopy (EIS) was employed for the detection of CCCVd sequence with the use of potassium ferricyanide (K3[Fe(CN)6]). Recognition of the RNA analytes was achieved via the significant increase in resistivity for the double stranded DNA, as compared to single-stranded DNA. The PSE-G/ZnO enhanced aptamer-based biosensor exhibited higher sensitivity than the bare biosensor, attributing to the synergistic effect of high electrical conductivity of graphene and good electroactive property of ZnO.

Keywords: aptamer-based biosensor, graphene/zinc oxide nanocomposite, green synthesis, screen printed carbon electrode

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Authors: Shivaji M. Sonawane, N. B. Chaure

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ZnTe is direct band gap, the P-type semiconductor with the high absorption coefficient of the order of 104cm-1 is suitable for solar cell development. It can be used as a low resistive ohmic contact to CdS/CdTe or tandem solar cell application. ZnTe and Cu-ZnTe thin film have been electrochemically synthesized on to fluorine-doped tin oxide coated glass substrates using three electrode systems containing Ag/AgCl, graphite and FTO as reference, counter and working electrode respectively were used to deposit the thin films. The aqueous electrolytic solution consist of 0.5M TeO2, 0.2M ZnSO4, and 0.1M Na3C6H5O7:2H2O, 0.1MC6H8O7:H2O and 0.1mMCuSO4 with PH 2.5 at room temperature was used. The reaction mechanism is studied in the cyclic voltammetry to identify the deposition potentials of ZnTe and Cu-ZnTe.The potential was optimized in the range -0,9 to -1,1 V. Vs Ag/AgCl reference electrode. The effect of deposition potential on the structural properties was studied by using X-ray diffraction. The X-ray diffraction result reveled cubic crystal structure of ZnTe with preferential (111) orientation with cubic structure. The surface morphology and film composition were analyzed by means of Scanning electron microscopy (SEM) and Energy Dispersive Analysis of X- Rays (EDAX). The optical absorption measurement has been analyzed for the band gap determination of deposited layers about 2.26 eV by UV-Visible spectroscopy. The drastic change in resistivity has been observed due to incorporation of copper probably due to the diffusion of Cu into grain boundaries.

Keywords: ohmic back contact, zinc telluride, electrodeposition, photovoltaic devices

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Authors: Anna Vanderbruggen, Kai Bachmann, Martin Rudolph, Rodrigo Serna

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Recycling of lithium-ion batteries has attracted a lot of attention in recent years and focuses primarily on valuable metals such as cobalt, nickel, and lithium. Despite the growth in graphite consumption and the fact that it is classified as a critical raw material in the European Union, USA, and Australia, there is little work focusing on graphite recycling. Thus, graphite is usually considered waste in recycling treatments, where graphite particles are concentrated in the “black mass”, a fine fraction below 1mm, which also contains the foils and the active cathode particles such as LiCoO2 or LiNiMnCoO2. To characterize the material, various analytical methods are applied, including X-Ray Fluorescence (XRF), X-Ray Diffraction (XRD), Atomic Absorption Spectrometry (AAS), and SEM-based automated mineralogy. The latter consists of the combination of a scanning electron microscopy (SEM) image analysis and energy-dispersive X-ray spectroscopy (EDS). It is a powerful and well-known method for primary material characterization; however, it has not yet been applied to secondary material such as black mass, which is a challenging material to analyze due to fine alloy particles and to the lack of an existing dedicated database. The aim of this research is to characterize the black mass depending on the metals recycling process in order to understand the liberation mechanisms of the active particles from the foils and their effect on the graphite particle surfaces and to understand their impact on the subsequent graphite flotation. Three industrial processes were taken into account: purely mechanical, pyrolysis-mechanical, and mechanical-hydrometallurgy. In summary, this article explores various and common challenges for graphite and secondary material characterization.

Keywords: automated mineralogy, characterization, graphite, lithium ion battery, recycling

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Authors: M. Pilar Valles-gonzalez, Alejandro Gonzalez Meije, Ana Pastor Muro, Maria Garcia-Martinez, Beatriz Gonzalez Caballero

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This paper studies a failure case of a fuel pressure supply tube from an aircraft engine. Multiple fracture cases of the fuel pressure control tube from aircraft engines have been reported. The studied set was composed of the mentioned tube, a welded connecting pipe, where the fracture has been produced, and a union nut. The fracture has been produced in one most critical zones of the tube, in a region next to the supporting body of the union nut to the connector. The tube material was X6CrNiTi18-10, an austenitic stainless steel. Chemical composition was determined using an X-Ray fluorescence spectrometer (XRF) and combustion equipment. Furthermore, the material has been mechanical, by hardness test, and microstructural characterized using a stereomicroscope and an optical microscope. The results confirmed that it is within specifications. To determine the macrofractographic features, a visual examination and a stereo microscope of the tube fracture surface have been carried out. The results revealed a tube plastic macrodeformation, surface damaged, and signs of a possible corrosion process. Fracture surface was also inspected by scanning electron microscopy (FE-SEM), equipped with a microanalysis system by X-ray dispersive energy (EDX), to determine the microfractographic features in order to find out the failure mechanism involved in the fracture. Fatigue striations, which are typical from a progressive fracture by a fatigue mechanism, have been observed. The origin of the fracture has been placed in defects located on the outer wall of the tube, leading to a final overload fracture.

Keywords: aircraft engine, fatigue, FE-SEM, fractography, fracture, fuel tube, microstructure, stainless steel

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Authors: Muhammad Qadir, Yuncang Li, Cuie Wen

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Surface properties such as topography and physicochemistry of metallic implants determine the cell behavior. The surface of titanium (Ti)-based implant can be modified to enhance the bioactivity and biocompatibility. In this study, a self-organized titania–niobium pentoxide–zirconia (TiO₂–Nb₂O₅–ZrO₂) nanotubular layer on β phase Ti35Zr28Nb alloy was fabricated via electrochemical anodization. Energy-dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and water contact angle measurement techniques were used to investigate the nanotubes dimensions (i.e., the inner and outer diameters, and wall thicknesses), microstructural features and evolution of the hydrophilic properties. The in vitro biocompatibility of the TiO₂–Nb₂O₅–ZrO₂ nanotubes (NTs) was assessed by using osteoblast cells (SaOS2). Influence of anodization parameters on the morphology of TiO₂–Nb₂O₅–ZrO₂ NTs has been studied. The results indicated that the average inner diameter, outer diameter and the wall thickness of the TiO₂–Nb₂O₅–ZrO₂ NTs were ranged from 25–70 nm, 45–90 nm and 5–13 nm, respectively, and were directly influenced by the applied voltage during anodization. The average inner and outer diameters of NTs increased with increasing applied voltage, and the length of NTs increased with increasing anodization time and water content of the electrolyte. In addition, the size distribution of the NTs noticeably affected the hydrophilic properties and enhanced the biocompatibility as compared with the uncoated substrate. The results of this study could be considered for developing nano-scale coatings for a wide range of biomedical applications.

Keywords: Titanium alloy, TiO₂–Nb₂O₅–ZrO₂ nanotubes, anodization, surface wettability, biocompatibility

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Authors: M. Cabuk, M. Yavuz, T. A. Yesil, H. I. Unal

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Electrorheological (ER) fluids are a class of smart materials exhibiting reversible changes in their rheological and mechanical properties under an applied electric field (E). ER fluids generally are composed of polarisable solid particles dispersed in non-conducting oil. ER fluids are fluids which exhibit. The resistance to motion of the ER fluid can be controlled by adjusting the applied E, due to their fast and reversible changes in their rheological properties presence of E. In this study, a series of chitosan/expanded perlite (CS/EP) composites with different chitosan mass fractions (10%, 20%, and 50%) was used. Characterizations of the composites were carried out by Fourier Transform Infrared (FTIR), X-ray diffraction (XRD) and Scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX) techniques. Antisedimentation stability and dielectric properties of the composites were also determined. The effects of volume fraction, electric field strength, shear rate, shear stress, and temperature onto ER properties of the CS/EP composite particles dispersed in silicone oil (SO) were investigated in detail. Vibration damping behavior of the CS/EP composites were determined as a function of frequence, storage (Gʹ) and loss (Gʹ ʹ) moduli. It was observed that ER response of the CS/EP/SO ER fluids increased with increasing electric field strength and exhibited the typical shear thinning non-Newtonian viscoelastic behaviors with increasing shear rate. The maximum yield stress was obtained with 1250 Pa under E = 3 kV/mm. Further, the CS/EP/SO ER fluids were observed to sensitive to vibration control by showing reversible viscosity enhancements (Gʹ > Gʹ ʹ). Acknowledgements: The authors thank the TÜBİTAK (214Z199) for the financial support of this work.

Keywords: chitosan, electrorheology, perlite, vibration control

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Authors: Victor Igwemezie, Ali Mehmanparast

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The correct knowledge of corrosion fatigue mechanism in marine steel is very important. This is because it enables the design, selection, and use of steels for offshore applications. It also supports realistic corrosion fatigue life prediction of marine structures. A study has been conducted to increase the understanding of corrosion fatigue mechanism in marine steels. The materials investigated are normalized and advanced S355 Thermomechanical control process (TMCP) steels commonly used in the design of offshore wind turbine support structures. The experimental study was carried out by conducting corrosion fatigue tests under conditions pertinent to offshore wind turbine operations, using the state of the art facilities. A careful microstructural study of the crack growth path was conducted using metallurgical optical microscope (OM), scanning electron microscope (SEM) and Energy Dispersive X-Ray Spectroscopy (EDX). The test was conducted on three subgrades of S355 steel: S355J2+N, S355G8+M and S355G10+M and the data compared with similar studies in the literature. The result shows that the ferrite-pearlite morphology primarily controls the corrosion-fatigue crack growth path in marine steels. A corrosion fatigue mechanism which relies on the hydrogen embrittlement of the grain boundaries and pearlite phase is used to explain the crack propagation behaviour. The crack growth trend in the Paris region of the da/dN vs. ΔK curve is used to explain the dependency of the corrosion-fatigue crack growth rate on the ferrite-pearlite morphology.

Keywords: corrosion-fatigue mechanism, fatigue crack growth rate, ferritic-pearlitic steel, microstructure, phase morphology

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Authors: A. E. Yakshin, D. Ijpes, J. M. Sturm, I. A. Makhotkin, M. D. Ackermann

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Applications like synchrotron optics, soft X-ray microscopy, X-ray astronomy, and wavelength dispersive X-ray fluorescence (WD-XRF) rely heavily on short- and ultra-short-period multilayer (ML) structures. In WD-XRF, ML serves as an analyzer crystal to disperse emission lines of light elements. The key requirement for the ML is to be highly reflective while also providing sufficient angular dispersion to resolve specific XRF lines. For these reasons, MLs with periods ranging from 1.0 to 2.5 nm are of great interest in this field. Due to the short period, the reflectance of such MLs is extremely sensitive to interface imperfections such as roughness and interdiffusion. Moreover, the thickness of the individual layers is only a few angstroms, which is close to the limit of materials to grow a continuous film. MLs with a period between 2.5 nm and 1.0 nm, combining tungsten (W) reflector with B₄C, Si, and Al spacers, were created and examined. These combinations show high theoretical reflectance in the full range from C-Kα (4.48nm) down to S-Kα (0.54nm). However, the formation of optically unfavorable compounds, intermixing, and interface roughness result in limited reflectance. A variety of techniques, including diffusion barriers, seed layers, and ion polishing for sputter-deposited MLs, were used to address these issues. Diffuse scattering measurements, photo-electron spectroscopy analysis, and X-ray reflectivity measurements showed a noticeable reduction of compound formation, intermixing, and interface roughness. This also resulted in a substantial increase in soft X-ray reflectance for W/Si, W/B4C, and W/Al MLs. In particular, the reflectivity of 1 nm period W/Si multilayers at the wavelength of 0.84 nm increased more than 3-fold – propelling forward the applicability of such multilayers for shorter wavelengths.

Keywords: interface engineering, reflectance, short period multilayer structures, x-ray optics

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Authors: Olanrewaju Rotimi Bodede, Akinlabi Oyetunji

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Modeling the dry compressive strength of sodium silicate bonded kaolin refractory bricks was studied. The materials used for this research work included refractory clay obtained from Ijero-Ekiti kaolin deposit on coordinates 7º 49´N and 5º 5´E, sodium silicate obtained from the open market in Lagos on coordinates 6°27′11″N 3°23′45″E all in the South Western part of Nigeria. The mineralogical composition of the kaolin clay was determined using the Energy Dispersive X-Ray Fluorescence Spectrometer (ED-XRF). The clay samples were crushed and sieved using the laboratory pulveriser, ball mill and sieve shaker respectively to obtain 100 μm diameter particles. Manual pipe extruder of dimension 30 mm diameter by 43.30 mm height was used to prepare the samples with varying percentage volume of sodium silicate 5 %, 7.5 % 10 %, 12.5 %, 15 %, 17.5 %, 20% and 22.5 % while kaolin and water were kept at 50 % and 5 % respectively for the comprehensive test. The samples were left to dry in the open laboratory atmosphere for 24 hours to remove moisture. The samples were then were fired in an electrically powered muffle furnace. Firing was done at the following temperatures; 700ºC, 750ºC, 800ºC, 850ºC, 900ºC, 950ºC, 1000ºC and 1100ºC. Compressive strength test was carried out on the dried samples using a Testometric Universal Testing Machine (TUTM) equipped with a computer and printer, optimum compression of 4.41 kN/mm2 was obtained at 12.5 % sodium silicate; the experimental results were modeled with MATLAB and Origin packages using polynomial regression equations that predicted the estimated values for dry compressive strength and later validated with Pearson’s rank correlation coefficient, thereby obtaining a very high positive correlation value of 0.97.

Keywords: dry compressive strength, kaolin, modeling, sodium silicate

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Authors: Mohamed Gouda

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Antibacterial wound dressings based on cellulose nanofibers containing different metal nanoparticles (CMC-MNPs) were synthesized using an electrospinning technique. First, the composite of carboxymethyl cellulose containing different metal nanoparticles (CMC/MNPs), such as copper nanoparticles (CuNPs), iron nanoparticles (FeNPs), zinc nanoparticles (ZnNPs), cadmium nanoparticles (CdNPs) and cobalt nanoparticles (CoNPs) were synthesized, and finally, these composites were transferred to the electrospinning process. Synthesized CMC-MNPs were characterized using scanning electron microscopy (SEM) coupled with high-energy dispersive X-ray (EDX) and UV-visible spectroscopy used to confirm nanoparticle formation. The SEM images clearly showed regular flat shapes with semi-porous surfaces. All MNPs were well distributed inside the backbone of the cellulose without aggregation. The average particle diameters were 29-39 nm for ZnNPs, 29-33 nm for CdNPs, 25-33 nm for CoNPs, 23-27 nm for CuNPs and 22-26 nm for FeNPs. Surface morphology, water uptake and release of MNPs from the nanofibers in water and antimicrobial efficacy were studied. SEM images revealed that electrospun CMC-MNPs nanofibers are smooth and uniformly distributed without bead formation with average fiber diameters in the range of 300 to 450 nm. Fiber diameters were not affected by the presence of MNPs. TEM images showed that MNPs are present in/on the electrospun CMC-MNPs nanofibers. The diameter of the electrospun nanofibers containing MNPs was in the range of 300–450 nm. The MNPs were observed to be spherical in shape. The CMC-MNPs nanofibers showed good hydrophilic properties and had excellent antibacterial activity against the Gram-negative bacteria Escherichia coli and the Gram-positive bacteria Staphylococcus aureus.

Keywords: electrospinning technique, metal nanoparticles, cellulosic nanofibers, wound dressing

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Authors: T. Deepa, S. R. Inchara, S. V. Venkatesh, Seema Tharannum

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Concrete is the most widely used structural material. It is made using locally available materials. However, Concrete has low tensile strength and may crack in the early days with exothermic hydration. Bacillus subtilis bacteria that form endospores is the biological agent considered in this study for Biomineralization or MICP (Microbially Induced Calcite Precipitation) Technique and to address the increased Construction water demand, Recycled Grey Water which is obtained from STP of PES University, opted in place of Potable water. In this work, M30 grade conventional concrete is designed using OPC 53 grade cement, Manufactured Sand, Natural coarse aggregates, and Potable water. Conventional Concrete (CC), Bacterial Concrete with Potable water (BS), and Recycled Grey Water concrete (RGW) are the three different concrete specimens casted. Experimental studies such as the strength test and the surface hardness test are conducted on Conventional and Bacterial concrete samples after 7, 28, and 56 days of curing. Concrete cubes are subjected to a temperature of 50° C to investigate the effect of higher temperature. Cracked cube specimens are observed for Self-healing - as well as microstructure analysis with Scanning Electron Microscope (SEM), Energy Dispersive X-Ray Analysis (EDAX), and X-Ray Diffraction Analysis (XRD).Noticeable Calcium salt deposition is observed on the surface of BS and RGW cracked specimen. Surface hardness and EDAX test gave promising result on the advantage of using spore-forming bacteria in concrete. This is followed by the strength gain in Compression and Flexure. Results also indicate that Recycled Grey Water can be a substitute for Normal water in concrete.

Keywords: bacillus subtilis, bacterial concrete, recycled grey water, self-healing, surface hardness of concrete

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Authors: Ricky Saputra, Rashmi Walvekar, Mohammad Khalid, Kaveh Shahbaz, Suganti Ramarad

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This particular study of interest aims to study the effect of coupling ultrasonic treatment with eutectic solvents in devulcanization process of waste rubber tyre. Specifically, three different types of Deep Eutectic Solvents (DES) were utilized, namely ChCl:Urea (1:2), ChCl:ZnCl₂ (1:2) and ZnCl₂:urea (2:7) in which their physicochemical properties were analysed and proven to have permissible water content that is less than 3.0 wt%, degradation temperature below 200ᵒC and freezing point below 60ᵒC. The mass ratio of rubber to DES was varied from 1:20-1:40, sonicated for 1 hour at 37 kHz and heated at variable time of 5-30 min at 180ᵒC. Energy dispersive x-rays (EDX) results revealed that the first two DESs give the highest degree of sulphur removal at 74.44 and 76.69% respectively with optimum heating time at 15 minutes whereby if prolonged, reformation of crosslink network would be experienced. Such is supported by the evidence shown by both FTIR and FESEM results where di-sulfide peak reappears at 30 minutes and morphological structures from 15 to 30 minutes change from smooth with high voidage to rigid with low voidage respectively. Furthermore, TGA curve reveals similar phenomena whereby at 15 minutes thermal decomposition temperature is at the lowest due to the decrease of molecular weight as a result of sulphur removal but increases back at 30 minutes. Type of bond change was also analysed whereby it was found that only di-sulphide bond was cleaved and which indicates partial-devulcanization. Overall, the results show that DES has a great potential to be used as devulcanizing solvent.

Keywords: crosslink network, devulcanization, eutectic solvents, reformation, ultrasonic

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Authors: A. Fernandez Zuvich, I. Gana Watkins, H. Zolotucho, H. Troiani, A. Caneiro, M. Prado, A. L. Soldati

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The study of actinide nanoparticles (NPs) has attracted the attention of the scientific community not only because the lack of information about their ecotoxicological effects but also because the use of NPs could open a new way in the production of nuclear energy. Indeed, it was recently demonstrated that UO2 NPs sintered pellets exhibit closed porosity with improved fission gas retention and radiation-tolerance , ameliorated mechanical properties, and less detriment of the thermal conductivity upon use, making them an interesting option for new nuclear fuels. In this work, we used a combination of diffraction and microscopy tools to characterize the morphology, the crystalline structure and the composition of UO2 nanoparticles doped with 10%wt Gd2O3. The particles were synthesized by a modified sol-gel method at low temperatures. X-ray Diffraction (XRD) studies determined the presence of a unique phase with the cubic structure and Fm3m spatial group, supporting that Gd atoms substitute U atoms in the fluorite structure of UO2. In addition, Field Emission Gun Scanning (FEG-SEM) and Transmission (FEG-TEM) Electron Microscopy images revealed the presence of micrometric agglomerates of nanoparticles, with rounded morphology and an average crystallite size < 50 nm. Energy Dispersive Spectroscopy (EDS) coupled to TEM determined the presence of Gd in all the analyzed crystallites. Besides, FEG-SEM-EDS showed a homogeneous concentration distribution at the micrometer scale indicating that the small size of the crystallites compensates the variation in composition by averaging a large number of crystallites. These techniques, as combined tools resulted thus essential to find out details of morphology and composition distribution at the sub-micrometer scale, and set a standard for developing and analyzing nanoparticulated nuclear fuels.

Keywords: actinide nanoparticles, burnable poison, nuclear fuel, sol-gel

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Authors: A. Cerrato Casado, C. Guigou, P. Jean

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In this investigation, the particle swarm optimization (PSO) algorithm is used to perform the inversion of the dispersion curves in the spectral analysis of surface waves (SASW) method. This inverse problem usually presents complicated solution spaces with many local minima that make difficult the convergence to the correct solution. PSO is a metaheuristic method that was originally designed to simulate social behavior but has demonstrated powerful capabilities to solve inverse problems with complex space solution and a high number of variables. The dispersion curve of the synthetic soils is constructed by the vertical flexibility coefficient method, which is especially convenient for soils where the stiffness does not increase gradually with depth. The reason is that these types of soil profiles are not normally dispersive since the dominant mode of Rayleigh waves is usually not coincident with the fundamental mode. Multiple synthetic soil profiles have been tested to show the characteristics of the convergence process and assess the accuracy of the final soil profile. In addition, the inversion procedure is applied to multiple real soils and the final profile compared with the available information. The combination of the vertical flexibility coefficient method to obtain the dispersion curve and the PSO algorithm to carry out the inversion process proves to be a robust procedure that is able to provide good solutions for complex soil profiles even with scarce prior information.

Keywords: dispersion, inverse problem, particle swarm optimization, SASW, soil profile

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Authors: Li Maksym, Prabhakar M. N., Jung-Il Song

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In this study, a flame retardant and hydrophobic cotton textile were prepared by utilizing a renewable halogen-free bio-based solution based on chitosan, urea, and phytic acid, named bio-flame retardant liquid (BFL), through facile dip-coating technology. Deposition of BFL on the surface of the cotton was confirmed by Fourier-transform infrared spectroscopy and scanning electron microscope coupled with energy-dispersive X-ray spectrometer. Thermal and flame retardant properties of the cottons were studied with thermogravimetric analysis, differential scanning calorimetry, vertical flame test, cone calorimeter test. Only with 8.8% of dry weight gain treaded cotton showed self-extinguish properties during fire test. Cone calorimeter test revealed a reduction of peak heat release rate from 203.2 to 21 kW/m2 and total heat release from 20.1 to 2.8 MJ/m2. Incidentally, BFL remarkably improved the thermal stability of flame retardant cotton from expressed in an enhanced amount of char at 700 °C (6.7 vs. 33.5%). BFL initiates the formation of phosphorous and silica contain char layer whichrestrains the propagation of heat and oxygen to unburned materialstrengthen by the liberation of non-combustible gases, which reduce the concentration of flammable volatiles and oxygen hence reducing the flammability of cotton. In addition, hydrophobicity and specific ignition test for upholstery application were performed. In conjunction, the proposed flame retardant cotton is potentially translatable to be utilized as upholstery materials in public transport.

Keywords: cotton farbic, flame retardancy, surface coating, intumescent mechanism

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Authors: Apichet Boonsoong

Abstract:

In the Chanthaburi-Trat basalts, xenoliths are composed of essentially ultramafic xenoliths (particularly spinel lherzolite) with a few of an aggregate of feldspar. Some 19 ultramafic xenoliths were collected from 13 different locations. They range in size from 3.5 to 60mm across. Most are weathered and oxidized on the surface but fresh samples are obtained from cut surfaces. Chemical analyses were performed on carbon-coated polished thin sections using a fully automated CAMECA SX-50 electron microprobe (EMPA) in wavelength-dispersive mode. In thin section, they are seen to consist of variable amounts of olivine, clinopyroxene, orthopyroxene with minor spinel and plagioclase, and are classed as lherzolite. Modal compositions of the ultramafic nodules vary with olivine (60-75%), clinopyroxene (20-30%), orthopyroxene (0-15%), minor spinel (1-3%) and plagioclase (<1%). The essential minerals form an equigranular, medium- to coarse-grained, granoblastic texture, and all are in mutual contact indicating attainment of equilibrium. Reaction rims are common along the nodule margins and in some are also present along grain boundaries. Zoning occurs in clinopyroxene, and to a lesser extent in orthopyroxene. The homogeneity of mineral compositions in lherzolite xenoliths suggests the attainment of equilibrium. The equilibration temperatures of these xenoliths are estimated to be in the range of 973 to 1063°C. Pressure estimates are not so easily obtained because no suitable barometer exists for garnet-free lherzolites and so an indirect method was used. The general mineral assemblage of the lherzolite xenoliths and the absence of garnet indicate a pressure range of approximately 12–19kbar, which is equivalent to depths approximately of 38 to 60km.

Keywords: chanthaburi-trat basalts, spinel lherzolite, xenoliths, 973 to 1063°C, 38 to 60km

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