Search results for: surface-enhanced raman spectroscopy (SERS)

Authors: José M. Liñeira Del Río, Ramón Rial, Khodor Nasser, María J.G. Guimarey

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The need to develop new lubricants that offer better anti-friction and anti-wear performance in internal combustion vehicles is one of the great challenges of lubrication in the automotive field. The addition of nanoparticles has emerged as a possible solution and, combined with the lubricating power of ionic liquids, may become one of the alternatives to reduce friction losses and wear of the contact surfaces in the conditions to which tribo-pairs are subjected, especially in the contact of the piston rings and the cylinder liner surface. In this study, the improvement in SAE 10W-40 engine oil tribological performance after the addition of magnesium oxide (MgO) nanoadditives and two different phosphonium-based ionic liquids (ILs) was investigated. The nanoparticle characterization was performed by means of transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, X-ray diffraction (XRD), and scanning electron microscopy (SEM). The tribological properties, friction coefficients and wear parameters of the formulated oil modified with 0.01 wt.% MgO and 1 wt.% ILs compared with the neat 10W-40 oil were performed and analyzed using a ball-on-three-pins tribometer and a 3D optical profilometer, respectively. Further analysis on the worn surface was carried out by Raman spectroscopy and SEM microscopy, illustrating the formation of the protective IL and MgO tribo-films as hybrid additives. In friction tests with sliding steel-steel tribo-pairs, IL3-based hybrid nanolubricant decreased the friction coefficient and wear volume by 7% and 59%, respectively, in comparison with the neat SAE 10W-40, while the one based on IL1 only achieved a reduction of these parameters by 6% and 39%, respectively. Thus, the tribological characterization also revealed that the MgO and IL3 addition has a positive synergy over the commercial lubricant, adequately meeting the requirements for their use in internal combustion engines. In summary, this study has shown that the addition of ionic liquids to MgO nanoparticles can improve the stability and lubrication behavior of MgO nanolubricant and encourages more investigations on using nanoparticle additives with green solvents such as ionic liquids to protect the environment as well as prolong the lifetime of machinery. The improvement in the lubricant properties was attributed to the following wear mechanisms: the formation of a protective tribo-film and the ability of nanoparticles to fill out valleys between asperities, thereby effectively smoothing out the shearing surfaces.

Keywords: lubricant, nanoparticles, phosphonium-based ionic liquids, tribology

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Authors: Pervaiz Ahmad, Mayeen Uddin Khandaker, Yusoff Mohd Amin

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A unique cone-like morphologies of boron nitride microtubes with larger internal space and thin walls structure are synthesized in a dual zone quartz tube furnace at 1200 ° C with ammonia as a reaction atmosphere. The synthesized microtubes are found to have diameter in the range of 1 to ̴ 2 μm with walls thickness estimated from 10 – 100 nm. XPS survey shows N 1s and B 1s peaks at 398.7 eV and 191 eV that represent h-BN in the sample. Raman spectroscopy indicates a high intensity peak at 1372.53 (cm-1) that corresponds to the E2g mode of h-BN.

Keywords: BNMTs, synthesis, reaction atmosphere, growth

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Authors: Sarre Nzaba, Bulelwa Ntsendwana, Bekkie Mamba, Alex Kuvarega

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The discharge of azo dyes such as Brilliant black (BB) into the water bodies has carcinogenic and mutagenic effects on humankind and the ecosystem. Conventional water treatment techniques fail to degrade these dyes completely thereby posing more problems. Advanced oxidation processes (AOPs) are promising technologies in solving the problem. Anatase type nitrogen-platinum (N, Pt) co-doped TiO₂ photocatalysts were prepared by a modified sol-gel method using amine terminated polyamidoamine generation 1 (PG1) as a template and source of nitrogen. The resultant photocatalysts were characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X‐ray photoelectron spectroscopy (XPS), UV‐Vis diffuse reflectance spectroscopy, photoluminescence spectroscopy (PL), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy (RS), thermal gravimetric analysis (TGA). The results showed that the calcination atmosphere played an important role in the morphology, crystal structure, spectral absorption, oxygen vacancy concentration, and visible light photocatalytic performance of the catalysts. Anatase phase particles ranging between 9- 20 nm were also confirmed by TEM, SEM, and analysis. The origin of the visible light photocatalytic activity was attributed to both the elemental N and Pd dopants and the existence of oxygen vacancies. Co-doping imparted a shift in the visible region of the solar spectrum. The visible light photocatalytic activity of the samples was investigated by monitoring the photocatalytic degradation of brilliant black dye. Co-doped TiO₂ showed greater photocatalytic brilliant black degradation efficiency compared to singly doped N-TiO₂ or Pd-TiO₂ under visible light irradiation. The highest reaction rate constant of 3.132 x 10-2 min⁻¹ was observed for N, Pd co-doped TiO₂ (2% Pd). The results demonstrated that the N, Pd co-doped TiO₂ (2% Pd) sample could completely degrade the dye in 3 h, while the commercial TiO₂ showed the lowest dye degradation efficiency (52.66%).

Keywords: brilliant black, Co-doped TiO₂, polyamidoamine generation 1 (PAMAM G1), photodegradation

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Authors: Hamsasew Hankebo Lemago, Dóra Hessz, Tamás Igricz, Zoltán Erdélyi, , Imre Miklós Szilágyi

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Metal oxide inverse opals are a promising class of photocatalysts with a unique hierarchical structure. Atomic layer deposition (ALD) is a versatile technique for the synthesis of high-precision metal oxide thin films, including inverse opals. In this study, we report the synthesis of TiO₂, ZnO, and Al₂O₃ inverse opal and their composites photocatalysts using thermal or plasma-enhanced ALD. The synthesized photocatalysts were characterized using a variety of techniques, including scanning electron microscopy (SEM)-energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Raman spectroscopy, photoluminescence (PL), ellipsometry, and UV-visible spectroscopy. The results showed that the ALD-synthesized metal oxide inverse opals had a highly ordered structure and a tunable pore size. The PL spectroscopy results showed low recombination rates of photogenerated electron-hole pairs, while the ellipsometry and UV-visible spectroscopy results showed tunable optical properties and band gap energies. The photocatalytic activity of the samples was evaluated by the degradation of methylene blue under visible light irradiation. The results showed that the ALD-synthesized metal oxide inverse opals exhibited high photocatalytic activity, even under visible light irradiation. The composites photocatalysts showed even higher activity than the individual metal oxide inverse opals. The enhanced photocatalytic activity of the composites can be attributed to the synergistic effect between the different metal oxides. For example, Al₂O₃ can act as a charge carrier scavenger, which can reduce the recombination of photogenerated electron-hole pairs. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production.

Keywords: ALD, metal oxide inverse opals, photocatalysis, composites

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Authors: Raghvendra Singh Yadav, Ivo Kuritka, Jarmila Vilcakova, Pavel Urbanek, Michal Machovsky, David Skoda, Milan Masar

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The elastomer nanocomposites were synthesized by solution mixing method with an elastomer as a matrix and in situ thermally reduced graphene oxide (RGO) and spinel ferrite NiFe₂O₄ nanoparticles as filler. Spinel ferrite NiFe₂O₄ nanoparticles were prepared by the starch-assisted sol-gel auto-combustion method. The influence of filler on the microstructure, morphology, dielectric, electrical and magnetic properties of Reduced Graphene Oxide-Nickel Ferrite-Elastomer nanocomposite was characterized by X-ray diffraction, Raman spectroscopy, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, X-ray photoelectron spectroscopy, the Dielectric Impedance analyzer, and vibrating sample magnetometer. Scanning electron microscopy study revealed that the fillers were incorporated in elastomer matrix homogeneously. The dielectric constant and dielectric tangent loss of nanocomposites was decreased with the increase of frequency, whereas, the dielectric constant increases with the addition of filler. Further, AC conductivity was increased with the increase of frequency and addition of fillers. Furthermore, the prepared nanocomposites exhibited ferromagnetic behavior. This work was supported by the Ministry of Education, Youth and Sports of the Czech Republic – Program NPU I (LO1504).

Keywords: polymer-matrix composites, nanoparticles as filler, dielectric property, magnetic property

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Authors: Astrid Tannert, Anuradha Ramoji, Christina Ebert, Frederike Gladigau, Lorena Tuchscherr, Jürgen Popp, Ute Neugebauer

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Staphylococcus aureus is a facultative intracellular pathogen, which by entering host cells may evade immunologic host response as well as antimicrobial treatment. In that way, S. aureus can cause persistent intracellular infections which are difficult to treat. Depending on the strain, S. aureus may persist at different intracellular locations like the phagolysosome. The first barrier invading pathogens from the blood stream that they have to cross are the endothelial cells lining the inner surface of blood and lymphatic vessels. Upon proceeding from an acute to a chronic infection, intracellular pathogens undergo certain biochemical and structural changes including a deceleration of metabolic processes to adopt for long-term intracellular survival and the development of a special phenotype designated as small colony variant. In this study, the endothelial cell line Ea.hy 926 was used as a model for acute and chronic S. aureus infection. To this end, Ea.hy 926 cells were cultured on QIAscout™ Microraft Arrays, a special graded cell culture substrate that contains around 12,000 microrafts of 200 µm edge length. After attachment to the substrate, the endothelial cells were infected with GFP-expressing S. aureus for 3 weeks. The acute infection and the development of persistent bacteria was followed by confocal laser scanning microscopy, scanning the whole Microraft Array for the presence and for detailed determination of the intracellular location of fluorescent intracellular bacteria every second day. After three weeks of infection representative microrafts containing infected cells, cells with protruded infections and cells that did never show any infection were isolated and fixed for Raman micro-spectroscopic investigation. For comparison, also microrafts with acute infection were isolated. The acquired Raman spectra are correlated with the fluorescence microscopic images to give hints about a) the molecular alterations in endothelial cells during acute and chronic infection compared to non-infected cells, and b) metabolic and structural changes within the pathogen when entering a mode of persistence within host cells. We thank Dr. Ruth Kläver from QIAGEN GmbH for her support regarding QIAscout technology. Financial support by the BMBF via the CSCC (FKZ 01EO1502) and from the DFG via the Jena Biophotonic and Imaging Laboratory (JBIL, FKZ PO 633/29-1, BA 1601/10-1) is highly acknowledged.

Keywords: correlative image analysis, intracellular infection, pathogen-host adaption, Raman micro-spectroscopy

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Authors: Nabil Al-Zaqri

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Semiconductor photocatalysts with surface defects display incredible light absorption bandwidth, and these defects function as highly active sites for oxidation processes by interacting with the surface band structure. Accordingly, engineering the photocatalyst with surface oxygen vacancies will enhance the semiconductor nanostructure's photocatalytic efficiency. Herein, a CeO2₋ₓ nanostructure is designed under the influence of low-frequency ultrasonic waves to create surface oxygen vacancies. This approach enhances the photocatalytic efficiency compared to many heterostructures while keeping the intrinsiccrystal structure intact. Ultrasonic waves induce the acoustic cavitation effect leading to the dissemination of active elements on the surface, which results in vacancy formation in conjunction with larger surface area and smaller particle size. The structural analysis of CeO₂₋ₓ revealed higher crystallinity, as well as morphological optimization, and the presence of oxygen vacancies is verified through Raman, X-rayphotoelectron spectroscopy, temperature-programmed reduction, photoluminescence, and electron spinresonance analyses. Oxygen vacancies accelerate the redox cycle between Ce₄+ and Ce₃+ by prolongingphotogenerated charge recombination. The ultrasound-treated pristine CeO₂ sample achieved excellenthydrogen production showing a quantum efficiency of 1.125% and efficient organic degradation. Ourpromising findings demonstrated that ultrasonic treatment causes the formation of surface oxygenvacancies and improves photocatalytic hydrogen evolution and pollution degradation. Conclusion: Defect engineering of the ceria nanoparticles with oxygen vacancies was achieved for the first time using low-frequency ultrasound treatment. The U-CeO₂₋ₓsample showed high crystallinity, and morphological changes were observed. Due to the acoustic cavitation effect, a larger surface area and small particle size were observed. The ultrasound treatment causes particle aggregation and surface defects leading to oxygen vacancy formation. The XPS, Raman spectroscopy, PL spectroscopy, and ESR results confirm the presence of oxygen vacancies. The ultrasound-treated sample was also examined for pollutant degradation, where 1O₂was found to be the major active species. Hence, the ultrasound treatment influences efficient photocatalysts for superior hydrogen evolution and an excellent photocatalytic degradation of contaminants. The prepared nanostructure showed excellent stability and recyclability. This work could pave the way for a unique post-synthesis strategy intended for efficient photocatalytic nanostructures.

Keywords: surface defect, CeO₂₋ₓ, photocatalytic, water treatment, H₂ production

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Authors: Vasant Reddy, Shivani A. Singh, Pravin S. More

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In the present investigation, we demonstrated the fabrication of few-layers of graphene sheets with alkali metal i.e. Rb-G using chemical route method. The obtained materials were characterized by means of chemical, structural and electrical techniques, using the ultraviolet-visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and 4 points probe, respectively. The XRD studies were carried out to understand the phase of the samples where we found a sharp peak of Rb-G at 26.470. UV-Spectroscopy of Graphene and Rb-modified graphene samples shows the absorption peaks at ~248 nm and ~318 nm respectively. These analyses show that this modified material can be useful for gas sensing applications and to be used in diverse areas.

Keywords: chemical route, graphene, gas sensing, UV-spectroscopy

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Authors: S. K. M. Nzaba, H. H. Nyoni, B. Ntsendwana, B. B. Mamba, A. T. Kuvarega

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Azo dye effluents, released into water bodies are not only toxic to the ecosystem but also pose a serious impact on human health due to the carcinogenic and mutagenic effects of the compounds present in the dye discharge. Conventional water treatment methods such as adsorption, flocculation/coagulation and biological processes are not effective in completely removing most of the dyes and their natural degradation by-products. Advanced oxidation processes (AOPs) have proven to be effective technologies for complete mineralization of these recalcitrant pollutants. Therefore, there is a need for new technology that can solve the problem. Thus, this study examined the photocatalytic degradation of an azo dye brilliant black (BB) using non-metal/metal codoped TiO₂. N, Pt co-doped TiO₂ photocatalysts were prepared by a modified sol-gel method using amine-terminated polyamidoamine dendrimer generation 0 (PAMAM G0), amine-terminated polyamidoamine dendrimer generation 1 ( PAMAM G1) and hyperbranched polyethyleneimine (HPEI) as templates and source of nitrogen. Structural, morphological, and textural properties were evaluated using scanning electron microscopy coupled to energy dispersive X-ray spectroscopy (SEM/EDX), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction spectroscopy (XRD), X-ray photoelectron spectroscopy (XPS), thermal gravimetric analysis (TGA), Fourier- transform infrared (FTIR), Raman spectroscopy (RS), photoluminescence (PL) and ultra-violet /visible spectroscopy (UV-Vis). The synthesized photocatalysts exhibited lower band gap energies as compared to the Degussa P-25 revealing a red shift in band gap towards the visible light absorption region. Photocatalytic activity of N, Pt co-doped TiO₂ was measured by the reaction of photocatalytic degradation of brilliant black (BB) dye. The N, metal codoped TiO₂ containing 0.5 wt. % of the metal consisted mainly of the anatase phase as confirmed by XRD results of all three samples, with a particle size range of 13–30 nm. The particles were largely spherical and shifted the absorption edge well into the visible region. Band gap reduction was more pronounced for the N, Pt HPEI (Pt 0.5 wt. %) codoped TiO₂ compared to PAMAM G0 and PAMAM G1. Consequently, codoping led to an enhancement in the photocatalytic activity of the materials for the degradation of brilliant black (BB).

Keywords: codoped TiO₂, dendrimer, photodegradation, wastewater

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Authors: Yi-Hao Pai, Wen-Feng Chen

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The planting area of Pomelo in Hualien, Taiwan amounts to thousands of hectares. Especially in the blooming season of Pomelo, it is an important producing area for Pomelo honey, and it is also a good test field for promoting the "Under-forest Economy". However, in the current Pomelo garden planting and management operations, the large amount of agricultural waste generated by the pruning of the branches causes environmental sanitation concerns, which can lead to the hiding of pests or the infection of the Pomelo tree, and indirectly increase the health risks of bees. Therefore, how to deal with the pruning of the branches and avoid open burning is a topic of social concern in recent years. In this research, afeasibility study evaluating energy conversion efficiency through agricultural waste gasification from the Pomelo garden, Taiwan, is demonstrated. we used a high-temperature gasifier to convert the pruning of the branches into syngas and biochar. In terms of syngas composition and calorific value assessment, we use the biogas monitoring system for analysis. Then, we used Raman spectroscopy and electron microscopy (EM) to diagnose the microstructure and surface morphology of biochar. The results indicate that the 1 ton of pruning of the branches can produce 1797.03m3 of syngas, corresponding to a calorific value of 9.1MJ/m3. The main components of the gas include CH4, H2, CO, and CO2, and the corresponding gas composition ratio is 16.8%, 7.1%, 13.7%, and 24.5%. Through the biomass syngas generator with a conversion efficiency of 30% for power generation, a total of 1,358kWh can be obtained per ton of pruning of the branches. In the research of biochar, its main characteristics in Raman spectroscopy are G bands and D bands. The first-order G and D bands are at 1580 and 1350 cm⁻¹, respectively. The G bands originates from the in-plane tangential stretching of the C−C bonds in the graphitic structure, and theD band corresponds to scattering from local defects or disorders present in carbon. The area ratio of D and G peaks (D/G) increases with the decrease of reaction temperature. The larger the D/G, the higher the defect concentration and the higher the porosity. This result is consistent with the microstructure displayed by SEM. The study is expected to be able to reuse agricultural waste and promote the development of agricultural and green energy circular economy.

Keywords: agricultural waste, gasification, energy conversion, pomelo garden

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Authors: Hasnaa Benchorfi

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The Tellurite glasses exhibit interesting properties, notably their low melting point (700-900°C), high refractive index (≈2), high transparency in the infrared region (up to 5−6 μm), interesting linear and non-linear optical properties and high rare earth ions solubility. These properties give tellurite glasses a great interest in various optical applications. Transparent ceramics present advantages compared to glasses, such as improved mechanical, thermal and optical properties. But, the elaboration process of these ceramics requires complex sintering conditions. The full crystallization of glass into transparent ceramics is an alternative to circumvent the technical challenges related to the ceramics obtained by conventional processing. In this work, a crystallization study of a specific glass composition in the system TeO2-Ta2O5-Bi2O3 shows structural transitions from the glass to the stabilization of an unreported anti-glass phase to a transparent ceramic upon heating. An anti-glass is a material with a cationic long-range order and a disordered anion sublattice. Thus, the X-ray diffraction patterns show sharp peaks, while the Raman bands are broad and similar to those of the parent glass. The structure and microstructure of the anti-glass and corresponding ceramic were characterized by Powder X-Ray Diffraction, Electron Back Scattered Diffraction, Transmission Electron Microscopy and Raman spectroscopy. The optical properties of the Er3+-doped samples are also discussed.

Keywords: glass, congruent crystallization, anti-glass, glass-ceramic, optics

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Authors: Yongde Xia, Laicong Deng, Zhuxian Yang

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Developing cost-effective electrocatalysts for oxygen reduction reaction (ORR), oxygen evolution reaction (OER) and hydrogen evolution reaction (HER) is vital in energy conversion and storage applications. Herein, we report a simple method for the synthesis of graphene-reinforced cobalt sulfide/carbon nanocomposites and the evaluation of their electrocatalytic performance for typical electrocatalytic reactions. Nanocomposites of cobalt sulfide embedded in N, S co-doped porous carbon and graphene (CoS@C/Graphene) were generated via simultaneous sulfurization and carbonization of one-pot synthesized graphite oxide-ZIF-67 precursors. The obtained CoS@C/Graphene nanocomposite was characterized by X-ray diffraction, Raman spectroscopy, Thermogravimetric analysis-Mass spectroscopy, Scanning electronic microscopy, Transmission electronic microscopy, X-ray photoelectron spectroscopy and gas sorption. It was found that cobalt sulfide nanoparticles were homogenously dispersed in the in-situ formed N, S co-doped porous carbon/Graphene matrix. The CoS@C/10Graphene composite not only shows excellent electrocatalytic activity toward ORR with high onset potential of 0.89 V, four-electron pathway and superior durability of maintaining 98% current after continuously running for around 5 hours, but also exhibits good performance for OER and HER, due to the improved electrical conductivity, increased catalytic active sites and connectivity between the electrocatalytic active cobalt sulfide and the carbon matrix. This work offers a new approach for the development of novel multifunctional nanocomposites for the next generation of energy conversion and storage applications.

Keywords: MOF derivative, graphene, electrocatalyst, oxygen reduction reaction, oxygen evolution reaction, hydrogen evolution reaction

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Authors: Mandlenkosi G. R. Mahlobo, Peter A. Olubambi, Philippe Refait

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The aim of this study was to use voltammetry as a method to understand the behaviour of steel in unsaturated soil in the presence of cathodic protection (CP). Three carbon steel coupons were buried in artificial soil wetted at 65-70% of saturation for 37 days. All three coupons were left at open circuit potential (OCP) for the first seven days in the unsaturated soil before CP, which was only applied on two of the three coupons at the protection potential -0.8 V vs Cu/CuSO₄ for the remaining 30 days of the experiment. Voltammetry was performed weekly on the coupon without CP, while electrochemical impedance spectroscopy (EIS) was performed daily to monitor and correct the applied CP potential from the ohmic drop. Voltammetry was finally performed on the last day on the coupons under CP. All the voltammograms were modeled with mathematical equations in order to compute the electrochemical parameters and subsequently deduced the corrosion rate of the steel coupons. For the coupon without CP, the corrosion rate was determined at 300 µm/y. For the coupons under CP, the residual corrosion rate under CP was estimated at 12 µm/y while the corrosion rate of the coupons, after interruption of CP, was estimated at 25 µm/y. This showed that CP was efficient due to two effects: a direct effect from the decreased potential and an induced effect associated with the increased interfacial pH that promoted the formation of a protective layer on the steel surface.

Keywords: carbon steel, cathodic protection, voltammetry, unsaturated soil, Raman spectroscopy

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Authors: Irina Veselova, Maria Makedonskaya, Olga Eremina, Alexandr Sidorov, Eugene Goodilin, Tatyana Shekhovtsova

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Such catecholamines as dopamine, norepinephrine, and epinephrine are the principal neurotransmitters in the sympathetic nervous system. Catecholamines and their metabolites are considered to be important markers of socially significant diseases such as atherosclerosis, diabetes, coronary heart disease, carcinogenesis, Alzheimer's and Parkinson's diseases. Currently, neurotransmitters can be studied via electrochemical and chromatographic techniques that allow their characterizing and quantification, although these techniques can only provide crude spatial information. Besides, the difficulty of catecholamine determination in biological materials is associated with their low normal concentrations (~ 1 nM) in biomaterials, which may become even one more order lower because of some disorders. In addition, in blood they are rapidly oxidized by monoaminooxidases from thrombocytes and, for this reason, the determination of neurotransmitter metabolism indicators in an organism should be very rapid (15—30 min), especially in critical states. Unfortunately, modern instrumental analysis does not offer a complex solution of this problem: despite its high sensitivity and selectivity, HPLC-MS cannot provide sufficiently rapid analysis, while enzymatic biosensors and immunoassays for the determination of the considered analytes lack sufficient sensitivity and reproducibility. Fluorescent and SERS-sensors remain a compelling technology for approaching the general problem of selective neurotransmitter detection. In recent years, a number of catecholamine sensors have been reported including RNA aptamers, fluorescent ribonucleopeptide (RNP) complexes, and boronic acid based synthetic receptors and the sensor operated in a turn-off mode. In this work we present the fluorescent and SERS turn-on sensor systems based on the bio- or chemorecognizing nanostructured films {chitosan/collagen-Tb/Eu/Cu-nanoparticles-indicator reagents} that provide the selective recognition, visualization, and sensing of the above mentioned catecholamines on the level of nanomolar concentrations in biomaterials (cell cultures, tissue etc.). We have (1) developed optically transparent porous films and gels of chitosan/collagen; (2) ensured functionalization of the surface by molecules-'recognizers' (by impregnation and immobilization of components of the indicator systems: biorecognizing and auxiliary reagents); (3) performed computer simulation for theoretical prediction and interpretation of some properties of the developed materials and obtained analytical signals in biomaterials. We are grateful for the financial support of this research from Russian Foundation for Basic Research (grants no. 15-03-05064 a, and 15-29-01330 ofi_m).

Keywords: biomaterials, fluorescent and SERS-recognition, neurotransmitters, solid-phase turn-on sensor system

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Authors: Venkataraman Sivasankar, Kiyoshi Omine, Hideaki Sano

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The leaching of fluoride from Plaster Board Waste (PBW) is quite feasible in soil and water environments. The Ministry of Environment, Japan recommended the standard limit of 0.8 mgL⁻¹ or less for fluoride. Although the utilization of PBW as a substitute for cement is rather meritorious, its fluoride leaching behavior deteriorates the quality of soil and water and therefore envisaged as a demerit. In view of this fluoride leaching problem, the present research is focused on immobilizing fluoride in PBW. The immobilization experiments were conducted with four chemical systems operated by DAHP (diammonium hydrogen phosphate) and phosphoric acid carbonization of bamboo mass coupled with certain inorganic reactions using reagents such as calcium hydroxide, sodium hydroxide, and aqueous ammonia. The fluoride immobilization was determined after shaking the reactor contents including the plaster board waste for 24 h at 25˚C. In the DAHP system, the immobilization of fluoride was evident from the leaching of fluoride in the range 0.071-0.12 mgL⁻¹, 0.026-0.14 mgL⁻¹ and 0.068-0.12 mgL⁻¹ for the reaction temperatures at 30˚C, 50˚C, and 90˚C, respectively, with final pH of 6.8. The other chemical systems designated as PACCa, PACAm, and PACNa could immobilize fluoride in PBW, and the resulting solution was analyzed with the fluoride less than the Japanese environmental standard of 0.8 mgL⁻¹. In the case of PACAm and PACCa systems, the calcium concentration was found undetectable and witnessed the formation of phosphate compounds. The immobilization of fluoride was found inversely proportional to the increase in the volume of leaching solvent and dose of PBW. Characterization studies of PBW and the solid after fluoride immobilization was done using FTIR (Fourier transform infrared spectroscopy), Raman spectroscopy, FE-SEM ( Field Emission Scanning Electron Microscopy) with EDAX (Energy Dispersive Spectroscopy), XRD (X-ray diffraction), and XPS (X-ray photoelectron spectroscopy). The results revealed the formation of new calcium phosphate compounds such as apatite, monetite, and hydroxylapatite. The participation of such new compounds in fluoride immobilization seems indispensable through the exchange mechanism of hydroxyl and fluoride groups. Acknowledgment: First author thanks to Japanese Society for the Promotion of Science (JSPS) for the award of the fellowship (ID No. 16544).

Keywords: characterization, fluoride, immobilization, plaster board waste

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Authors: Syed W. Hasan, Zhiqun Tian

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Wet spinning provides a facile and economic route to fabricate graphene nanofibers (GFs) on mass scale. Nevertheless, the pristine GFs exhibit significantly low electrical and mechanical properties owing to stacked graphene sheets and weak inter-atomic bonding. In this report, we present highly conductive Ag-decorated-GFs (Ag/GFs). The SEM micrographs show Ag nanoparticles (NPs) (dia ~10 nm) are homogeneously distributed throughout the cross-section of the fiber. The Ag NPs provide a conductive network for the electrons flow raising the conductivity to 1.8(10^4) S/m which is 4 times higher than the pristine GFs. Our results surpass the conductivities of graphene fibers doped with CNTs, Nanocarbon, fullerene, and Cu. The chemical and structural attributes of Ag/GFs are further elucidated through XPS, AFM and Raman spectroscopy.

Keywords: Ag nanoparticles, Conductive fibers, Graphene, Wet spinning

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Authors: M. Barbouche, M. Hajji, H. Ezzaouia

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This project is a step to manufacture solar grade silicon. It consists in designing an electrical arc furnace in order to produce metallurgical silicon Mg-Si with mutually carbon and high purity of silica. It concerns, first, the development of a functional analysis, a mechanical design and thermodynamic study. Our study covers also, the design of the temperature control system and the design of the electric diagrams. The furnace works correctly. A Labview interface was developed to control all parameters and to supervise the operation of furnace. Characterization tests with X-ray technique and Raman spectroscopy allow us to confirm the metallurgical silicon production.

Keywords: arc furnace, electrical design, silicon manufacturing, regulation, x-ray characterization

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Authors: Suhaila Isaak, Yusmeeraz Yusof, Khairunnisa Mohd Yusof, Ahmad Safuan Abdul Rashid

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Soil fertility is commonly evaluated by soil macronutrients such as nitrate, potassium, and phosphorus contents. Optical spectroscopy is an emerging technology which is rapid and simple has been widely used in agriculture to measure soil fertility. For visible and near infrared absorption spectroscopy, the absorbed light level in is useful for soil macro-nutrient measurement. This is because the absorption of light in a soil sample influences sensitivity of the measurement. This paper reports the performance of visible and near infrared absorption spectroscopy in the 400–1400 nm wavelength range using light-emitting diode as the excitation light source to predict the soil macronutrient content of nitrate, potassium, and phosphorus. The experimental results show an improved linear regression analysis of various soil specimens based on the Beer–Lambert law to determine sensitivity of soil spectroscopy by evaluating the absorption of characteristic peaks emitted from a light-emitting diode and detected by high sensitivity optical spectrometer. This would denote in developing a simple and low-cost soil spectroscopy with light-emitting diode for future implementation.

Keywords: macronutrients absorption, optical spectroscopy, soil, absorption

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Authors: Azeez O. Idris, Benjamin O. Orimolade, Potlako J. Mafa, Alex T. Kuvarega, Usisipho Feleni, Bhekie B. Mamba

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We report a simple and cheaper method for the electrochemical detection of Se(IV) using carbon nanodots (CNDTs) prepared from oat. The carbon nanodots were synthesised by green and facile approach and characterised using scanning electron microscopy, high-resolution transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, and Raman spectroscopy. The CNDT was used to fabricate an electrochemical sensor for the quantification of Se(IV) in water. The modification of glassy carbon electrode (GCE) with carbon nanodots led to an increase in the electroactive surface area of the electrode, which enhances the redox current peak of [Fe(CN)₆]₃₋/₄‒ in comparison to the bare GCE. Using the square wave voltammetry, the detection limit and quantification limit of 0.05 and 0.167 ppb were obtained under the optimised parameters using deposition potential of -200 mV, 0.1 M HNO₃ electrolyte, electrodeposition time of 60 s, and pH 1. The results further revealed that the GCE-CNDT was not susceptible to many interfering cations except Cu(II) and Pb(II), and Fe(II). The sensor fabrication involves a one-step electrode modification and was used to detect Se(IV) in a real water sample, and the result obtained is in agreement with the inductively coupled plasma technique. Overall, the electrode offers a cheap, fast, and sensitive way of detecting selenium in environmental matrices.

Keywords: carbon nanodots, square wave voltammetry, nanomaterials, selenium, sensor

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Authors: Raghvendra Singh Yadav, Ivo Kuřitka, Jarmila Vilcakova, Pavel Urbánek, Michal Machovsky, Milan Masař, Martin Holek

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Herein, we reported the influence of La³⁺ substitution on structural, magnetic and dielectric properties of CoFe₂O₄ nanoparticles synthesized by starch-assisted sol-gel combustion method. X-ray diffraction pattern confirmed the formation of cubic spinel structure of La³⁺ ions doped CoFe₂O₄ nanoparticles. Raman and Fourier Transform Infrared spectroscopy study also confirmed cubic spinel structure of La³⁺ substituted CoFe₂O₄ nanoparticles. The field emission scanning electron microscopy study revealed that La³⁺ substituted CoFe2O4 nanoparticles were in the range of 10-40 nm. The magnetic properties of La³⁺ substituted CoFe₂O₄ nanoparticles were investigated by using vibrating sample magnetometer. The variation in saturation magnetization, coercivity and remanent magnetization with La³⁺ concentration in CoFe2O4 nanoparticles was observed. The variation of real and imaginary part of dielectric constant, tan δ, and AC conductivity were studied with change of concentration of La³⁺ ions in CoFe₂O₄ nanoparticles. The variation in optical properties was studied via UV-Vis absorption spectroscopy. Acknowledgment: This work was supported by the Ministry of Education, Youth and Sports of the Czech Republic – Program NPU I (LO1504).

Keywords: starch, sol-gel combustion method, nanoparticles, magnetic properties, dielectric properties

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Authors: Omar Omar, Yuan Jun, Hong Jinghua, Jin Chuanhong

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In this work molybdenum dioxide (MoO2) and sulphur powders are used to grow MoS2 mono layers at elevated temperatures T≥800 °C. Centimetre scale continues thin films with grain size up to 410 µm have been grown using chemical vapour deposition. To our best knowledge, these domains are the largest that have been grown so far. Advantage of our approach is not only because of the high quality films with large domain size one can produce, but also the procedure is potentially less hazardous than other methods tried. The thin films have been characterized using transmission electron microscopy (TEM), atomic force microscopy (AFM) and Raman spectroscopy.

Keywords: molybdenum disulphide (MoS2), monolayers, chemical vapour deposition (CVD), growth and characterization

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Authors: Hamsasew Hankebo Lemago, Dóra Hessz, Zoltán Erdélyi, Imre Miklós Szilágyi

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Metal oxide inverse opals are a unique class of photocatalysts with a hierarchical structure that mimics the natural opal gemstone. They are composed of a network of interconnected pores, which provides a large surface area and efficient pathways for the transport of light and reactants. Atomic layer deposition (ALD) is a versatile technique for the synthesis of high-precision metal oxide thin films, including inverse opals. ALD allows for precise control over the thickness, composition, and morphology of the synthesized films, making it an ideal technique for the fabrication of photocatalysts with tailored properties. In this study, we report the synthesis of TiO2, ZnO, and Al2O3 inverse opal photocatalysts using thermal or plasma-enhanced ALD. The synthesized photocatalysts were characterized using a variety of techniques, including scanning electron microscopy (SEM)-energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Raman spectroscopy, photoluminescence (PL), ellipsometry, and UV-visible spectroscopy. The results showed that the ALD-synthesized metal oxide inverse opals had a highly ordered structure and a tunable pore size. The PL spectroscopy results showed low recombination rates of photogenerated electron-hole pairs, while the ellipsometry and UV-visible spectroscopy results showed tunable optical properties and band gap energies. The photocatalytic activity of the samples was evaluated by the degradation of methylene blue under visible light irradiation. The results showed that the ALD-synthesized metal oxide inverse opals exhibited high photocatalytic activity, even under visible light irradiation. The composites photocatalysts showed even higher activity than the individual metal oxide inverse opals. The enhanced photocatalytic activity of the composites can be attributed to the synergistic effect between the different metal oxides. For example, Al2O3 can act as a charge carrier scavenger, which can reduce the recombination of photogenerated electron-hole pairs. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production. For example, they can be used to remove organic pollutants from wastewater, decompose harmful gases in the air, and produce hydrogen fuel from water.

Keywords: ALD, metal oxide inverse opals, composites, photocatalysis

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Authors: Hatem Diaf, Patrice Melinon, Antonio Pereira, Bernard Moine, Nicholas Blanchard, Florent Bourquard, Florence Garrelie, Christophe Donnet

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Glassy carbon exhibits excellent biological compatibility with live tissues meaning it has high potential for applications in life science. Moreover, glassy carbon has interesting properties including 'high temperature resistance', hardness, low density, low electrical resistance, low friction, and low thermal resistance. The structure of glassy carbon has long been a subject of debate. It is now admitted that glassy carbon is 100% sp2. This term is a little bit confusing as long sp2 hybridization defined from quantum chemistry is related to both properties: threefold configuration and pi bonding (parallel pz orbitals). Using plasma laser deposition of carbon clusters combined with pulsed nano/femto laser annealing, we are able to synthesize thin films of glassy carbon of good quality (probed by G band/ D disorder band ratio in Raman spectroscopy) without thermal post annealing. A careful inspecting of Raman signal, plasmon losses and structure performed by HRTEM (High Resolution Transmission Electron Microscopy) reveals that both properties (threefold and pi orbitals) cannot coexist together. The structure of the films is compared to models including schwarzites based from negatively curved surfaces at the opposite of onions or fullerene-like structures with positively curved surfaces. This study shows that a huge collection of porous carbon named vitreous carbon with different structures can coexist.

Keywords: glassy carbon, cluster deposition, coating, electronic structure

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Authors: Boda Sreenivas, Lyathakula Ravindranath, Kanugula Srishailam, Byru Venkatram Reddy

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Extensive research into the optimized structure and molecular properties of 3-Flouro-2-methylbenzoicacid(FMB), 3-Chloro-2-methoxybenzoicacid (CMB), and 3-Bromo-2-methylbenzoicacid (BMB) was carried out using FT-IR, FT-Raman and UV-Visible spectra, as well as theoretically using the DFT approach with B3LYPfunctional in conjunction with 6-311++G(d,p) basis set. The optimized structure was determined by evaluating torsional scans about free rotation bonds. Structure parameters, harmonic vibrational frequencies, potential energy distribution(PED), and infrared and Raman intensities were computed. The computational results from the DFT approach, such asFT-IR, FT-Raman, and UV-Visible spectra, were compared with the experimental results and found good agreement. Observed and calculated frequencies agreed with an rms error of 8.42, 6.60, and 6.95 cm-1 for FMB, CMB, and BMB, respectively. Unambiguous vibrational assignments were made for all fundamentals using PED and eigenvectors. The electronic HOMO-LUMO, H-bonding, and strong conjugative interactions across different molecular entities are discussed using experimental and simulated Ultraviolet-Visible spectra. The title molecules' molecular properties such as dipole moment, mean polarizability, and first-order hyperpolarizability, were calculated to study their non-linear optical (NLO) behavior. The chemical reactivity descriptors and mapped electrostatic surface potential (MESP) were also evaluated. Natural bond orbital (NBO) analysis was used to examine the stability of molecules resulting from hyperconjugative interactions and charge delocalization.

Keywords: ftir/raman spectra, DFT, NLO, homo-lumo, NBO, halogenated benzoic acids

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Authors: Kriangkrai Aranyarat

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The effect of N2 pretreatment on the catalytic activity of tungsten-based catalysts was investigated in the metathesis of ethylene and trans-2-butene at 450oC and atmospheric pressure. The presence of tungsten active species was confirmed by UV-Vis and Raman spectroscopy. Compared to the WO3-based catalysts treated in air, higher amount of WO42- tetrahedral species and lower amount of WO3 crystalline species were observed on the N2-treated ones. These contribute to the higher conversion of 2-butene and propylene selectivity during 10 h time-on-stream. Moreover, N2 treatment led to lower amount of coke formation as revealed by TPO of the spent catalysts.

Keywords: metathesis, pretreatment, propylene, tungsten

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Authors: Bharat Kumar, Deepak Kumar, Vijay Chaudhry

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Zirconium alloys are used as core components of nuclear reactors due to their high wear resistance, good corrosion properties, and good mechanical stability at high temperatures. Water flows inside the pressure tube through fuel claddings, which produces vibration of these core components and results in the wear of some components. Some components are subjected to the environment of coolant water containing LiOH which results in the corrosion of these components. The present work simulates some of these conditions to determine the failure mechanisms under these conditions and the effect of various parameters on them. Friction and wear experiments were performed varying the surrounding environment (room temperature, high temperature, and water submerged), duration, frequency, and displacement amplitude. Electrochemical corrosion experiments were performed by varying the concentration of LiOH in water. The worn and corroded surfaces were analyzed using scanning electron microscopy (SEM) to analyze the wear and corrosion mechanism and energy dispersive x-ray spectroscopy (EDS) and Raman spectroscopy to analyze the tribo-oxide layer formed during the wear and oxide layer formed during the corrosion. Wear increases with frequency and amplitude, and corrosion increases with LiOH concentration in water.

Keywords: zirconium alloys, wear, oxide layer, corrosion, EIS, linear polarization

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Authors: Indu Elizabeth

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Antimony/Multi Walled Carbon nano tube nanocomposite (Sb/MWCNT) is synthesized using ethylene glycol mediated reduction process. Binder free, self-supporting and flexible Sb/MWCNT nanocomposite paper has been prepared by employing the vacuum filtration technique. The samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy (RS), and thermal gravimetric analysis (TGA) to evaluate the structure of anode and tested for its performance in a Lithium rechargeable cell. Electrochemical measurements demonstrate that the Sb/MWCNT composite paper anode delivers a specific discharge capacity of ~400 mAh g-1 up to a current density of 100 mA g-1.

Keywords: antimony, lithium ion battery, multiwalled carbon nanotube, specific capacity

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Authors: Vanessa Romanovicz, Beatriz A. Berns, Stephen D. Carpenter, Deyse Carpenter

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This article deals with the carbon nanotubes (CNT) synthesized from a novel precursor, sugar cane and Anodic Aluminum Oxide (AAO). The objective was to produce CNTs to be used as catalyst supports for Proton Exchange Membranes. The influence of temperature, inert gas flow rate and concentration of the precursor is presented. The CNTs prepared were characterized using TEM, XRD, Raman Spectroscopy, and the surface area determined by BET. The results show that it is possible to form CNT from sugar cane by pyrolysis and the CNTs are the type multi-walled carbon nanotubes. The MWCNTs are short and closed at the two ends with very small surface area of SBET = 3.691m,/g.

Keywords: carbon nanotubes, sugar cane, fuel cell, catalyst support

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Authors: Marcia Silva, Jayme Kolarik, Brennon Garthwait, William Lee, Hai-Feng Zhang

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Adsorption of lead by a natural porous material was studied to establish a baseline for the removal of heavy metals from drinking and waste water. Samples were examined under different conditions such as solution pH, solution concentration, solution temperature, and exposure time. New materials with potentially enhanced adsorption properties were developed by functionalizing the surface of the natural porous material to fabricate graphene based coated and sulfide based treated porous material. The functionalized materials were characterized with Fourier Transform Infrared Spectroscopy (FTIR), Raman, Thermogravimetric Analysis (TGA) and Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS) techniques. Solution pH effect on removal efficiency has been investigated in acidic (pH = 4), neutral (pH = 6) and basic (pH = 10) pH levels. All adsorbent materials showed highest adsorption capacities at neutral pH levels. Batch experiment was employed to assess the efficacy for the removal of lead with the sorption kinetics and the adsorption isotherms being determined for the natural and treated porous materials. The addition of graphene-based and sulfide-based materials increased the lead removal capacity of the natural clean porous material. Theoretical calculations confirmed pseudo-second order model as kinetic mechanism for lead adsorption for all adsorbents.

Keywords: heavy metals, ion exchange, adsorption, water remediation

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Authors: Hanan Alenezi

Abstract:

Membrane performance depends on the kind of solvent used in preparation. A membrane made by Polyetherimide (PEI) was evaluated for gas separation using X-Ray Diffraction (XRD), Scanning electron microscope (SEM), and Energy Dispersive X-Ray Spectroscopy (EDS). The purity and the thickness are detected to evaluate the membrane in order to optimize PEI membrane preparation.

Keywords: Energy Dispersive X-Ray Spectroscopy (EDS), Membrane, Polyetherimide PEI, Scanning electron microscope (SEM), Solvent, X-Ray Diffraction (XRD)

Procedia PDF Downloads 184