Search results for: Scanning Electron Microscopy-Energy Dispersive Spectroscopy

Authors: K. Tomolya, D. Janovszky, A. Sycheva, M. Sveda, A. Roosz

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CuZrAl amorphous alloys have attracted high interest due to unique physical and mechanical properties, which can be enhanced by adding of Ni and Ti elements. It is known that this properties can be enhanced by crystallization of amorphous alloys creating nanocrystallines in the matrix. The present work intends to produce nanosized crystalline parti-cle reinforced amorphous matrix composite powders by crystallization of amorphous powders. As the first step the amorphous powders were synthe-tized by ball-milling of crystalline powders. (Cu49Zr45Al6) 80Ni10Ti10 and (Cu49Zr44Al7) 80Ni10Ti10 (at%) alloys were ball-milled for 12 hours in order to reach the fully amorphous structure. The impact en-ergy of the balls during milling causes the change of the structure in the powders. Scanning electron microscopical (SEM) images shows that the phases mixed first and then changed into a fully amorphous matrix. Furthermore, nanosized particles in the amorphous matrix were crystallized by heat treatment of the amorphous powders that was confirmed by TEM measurement. It was of importance to define the tem-perature when the amorphous phase starts to crystal-lize. Amorphous alloys have a special heating curve and characteristic temperatures, which can be meas-ured by differential scanning calorimetry (DSC). A typical DSC curve of an amorphous alloy exhibits an endothermic event characteristic of the equilibrium glass transition (Tg) and a distinct undercooled liquid region, followed by one or two exothermic events corresponding to crystallization processes (Tp). After measuring the DSC traces of the amorphous powders, the annealing temperatures should be determined between Tx and Tp. In our experiments several temperatures from the annealing temperature range were selected and de-pendency of crystallized nanoparticles fraction on their hardness was investigated.

Keywords: amorphous structure, composite, mechanical milling, powder, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), transmission electronmocroscopy (TEM)

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Authors: Shaeel A. Al Thabaiti, Sulaiman N. Basahel, Salem M. Bawaked, Mohamed Mokhtar

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Nanosheets for cobalt-layered double hydroxide (Co-Al-LDH)/GO were successfully synthesized with different Co:M g:Al ratios (0:3:1, 1.5:1.5:1, and 3:0:1). The layered double hydroxide structure and morphology were determined using x-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). Temperature prgrammed reduction (TPR) of Co-Al-LDH showed reduction peaks at lower temperature which indicates the ease reducibility of this particular sample. The thermal behaviour was studied using thermal graviemetric technique (TG), and the BET-surface area was determined using N2 physisorption at -196°C. The C-C coupling reaction was carried out over all the investigated catalysts. The Mg–Al LDH catalyst without Co ions is inactive, but the isomorphic substitution of Mg by Co ions (Co:Mg:Al = 1.5:1.5:1) in the cationic sheet resulted in 88% conversion of iodobenzene under reflux. LDH/GO hybrid is up to 2 times higher activity than for the unsupported LDH.

Keywords: adsorption, co-precipitation, graphene oxide, layer double hydroxide

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Authors: Adeyemi Isaac Sanusi, Gueguim E. B. Kana

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Nanoparticles have received attention of the scientific community due to their biotechnological potentials. They exhibit advantageous size, shape and concentration-dependent catalytic, stabilizing, immunoassays and immobilization properties. This study investigates the impact of metallic oxide nanoparticles (NPs) on ethanol production by Saccharomyces cerevisiae BY4743. Nine different nanoparticles were synthesized using precipitation method and microwave treatment. The nanoparticles synthesized were characterized by Fourier Transform Infra-Red spectroscopy (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Fermentation processes were carried out at varied NPs concentrations (0 – 0.08 wt%). Highest ethanol concentrations were achieved after 24 h using Cobalt NPs (5.07 g/l), Copper NPs (4.86 g/l) and Manganese NPs (4.74 g/l) at 0.01 wt% NPs concentrations, which represent 13%, 8.7% and 5.4% increase respectively over the control (4.47 g/l). The lowest ethanol concentration (0.17 g/l) was obtained when 0.08 wt% of Silver NPs was used. And lower ethanol concentrations were observed at higher NPs concentration. Ethanol concentration decrease after 24 h for all the processes. In all set up with NPs, the pH was observed to be stable and the stability was directly proportional to nanoparticles concentrations. These findings suggest that the presence of some of the NPs in the bioprocesses has catalytic and pH stabilizing potential. Ethanol production by Saccharomyces cerevisiae BY4743 was enhanced in the presence of Cobalt NPs, Copper NPs and Manganese NPs. Optimization study using response surface methodology (RSM) will further elucidate the impact of these nanoparticles on bioethanol production.

Keywords: agitation, bioethanol, nanoparticles concentration, optimization, pH value

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Authors: M. Al Nur, M. S. Kaiser

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Corrosion behaviour of hypereutectic Al-19Si automotive alloy in different pH=1, 3, 5, 7, 9, 11, and 13 environments was carried out using conventional gravimetric measurements and was complemented by resistivity, optical micrograph, scanning electron microscopy (SEM) and X-ray analyzer (EDX) investigations. Gravimetric analysis confirmed that the highest corrosion rate is shown at pH 13 followed by pH 1. Minimum corrosion occurs in the pH range of 3.0 to 11 due to establishment of passive layer on the surface. The highest corrosion rate at pH 13 is due to the presence of sodium hydroxide in the solution which dissolves the surface oxide film at a steady rate. At pH 1, it can be attributed that the presence of aggressive chloride ions serves to pick up the damage of the passive films at localized regions. With varying exposure periods by both, the environment complies with the normal corrosion rate profile that is an initial steep rise followed by a nearly constant value of corrosion rate. Resistivity increases in case of pH 1 solution for the higher pit formation and decreases at pH 13 due to formation of thin film. The SEM image of corroded samples immersed in pH 1 solution clearly shows pores on the surface and in pH 13 solution, and the corrosion layer seems more compact and homogenous and not porous.

Keywords: Al-Si alloy, corrosion, pH, resistivity, scanning electron microscopy (SEM)

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Authors: Abdelmajid Timoumi, Salah Alamri, Hatem Alamri

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TiO₂ Graphene Oxide (TiO₂-GO) nanocomposite was prepared using the spin coating technique of suspension of Graphene Oxide (GO) nanosheets and Titanium Tetra Isopropoxide (TIP). The prepared nanocomposites samples were characterized by X-ray diffractometer, Scanning Electron Microscope and Atomic Force Microscope to examine their structures and morphologies. UV-vis transmittance and reflectance spectroscopy was employed to estimate band gap energies. From the TiO₂-GO samples, a 0.25 μm thin layer on a piece of glass 2x2 cm was created. The X-ray diffraction analysis revealed that the as-deposited layers are amorphous in nature. The surface morphology images demonstrate that the layers grew in distributed with some spherical/rod-like and partially agglomerated TiGO on the surface of the composite. The Atomic Force Microscopy indicated that the films are smooth with slightly larger surface roughness. The analysis of optical absorption data of the layers showed that the values of band gap energy decreased from 3.46 eV to 1.40 eV, depending on the grams of GO doping. This reduction might be attributed to electron and/or hole trapping at the donor and acceptor levels in the TiO₂ band structure. Observed results have shown that the inclusion of GO in the TiO₂ matrix have exhibited significant and excellent properties, which would be promising for application in the photovoltaic application.

Keywords: titanium dioxide, graphene oxide, thin films, solar cells

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

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

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

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Authors: F. Kashanian, M. M. Masoudi, A. Akbari, A. Shamloo, M. R. Zand, S. S. Salehi

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Nano-sized materials present new opportunities in biology and medicine and they are used as biomedical tools for investigation, separation of molecules and cells. To achieve more effective cancer therapy, it is essential to select cancer cells exactly. This research suggests that using the antibody-functionalized nontoxic Arginine-doped magnetic nanoparticles (A-MNPs), has been prosperous in detection, capture, and magnetic separation of circulating tumor cells (CTCs) in tumor tissue. In this study, A-MNPs were synthesized via a simple precipitation reaction and directly immobilized Ep-CAM EBA-1 antibodies over superparamagnetic A-MNPs for Mucin BCA-225 in breast cancer cell. The samples were characterized by vibrating sample magnetometer (VSM), FT-IR spectroscopy, Tunneling Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM). These antibody-functionalized nontoxic A-MNPs were used to capture breast cancer cell. Through employing a strong permanent magnet, the magnetic separation was achieved within a few seconds. Antibody-Conjugated nontoxic Arginine-doped Fe₃O₄ nanoparticles have the potential for the future study to capture CTCs which are released from tumor tissue and for drug delivery, and these results demonstrate that the antibody-conjugated A-MNPs can be used in magnetic hyperthermia techniques for cancer treatment.

Keywords: tumor tissue, antibody, magnetic nanoparticle, CTCs capturing

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Authors: Gina Zavaleta-Espejo, Segundo R. Jáuregui-Rosas, Fanny V. Samanamud-Moreno, José Saldaña Jiménez, Anibal Felix-Quintero, Víctor Montero-Del Aguila, Elsi Mejía-Uriarte

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Vicugnapacos "alpaca" fabrics are considered special for their finesse, and the garments in the textile market are very luxurious. It has many special characteristics such as antiallergic, soft, hygroscopic, among others. In this sense, the research aimed to evaluate the antimicrobial activity of alpaca fabrics functionalized with silver nanoparticles on the bacteria Escherichia coli ATCC 25922 and Staphylococcus aureus ATCC 25923. For the functionalization of the fabrics, AgNO3 and different concentrations of trisodium citrate (TSC) 2, 6, and 10 mg. Tissue characterization was performed using Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). The determination of the antimicrobial activity of the alpaca tissues was made by the Kirby-Bauer method with alpaca tissue discs functionalized with silver nanoparticles, an experimental design was made in completely randomized blocks with three treatments and a negative control with three repetitions. The results showed that inhibition halos were formed for both bacteria, therefore, the functionalized tissues have a high antimicrobial activity, whose mechanism of action is attributed to the free radicals (ROS) generated by the nanoparticles that cause oxidative damage to the bacteria. proteins and lipids of the bacterial cell wall.

Keywords: antimicrobial, animal fibers, fabrics, functionalization, trisodium citrate

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Authors: Chetna Tyagi. G. B. V. S. Lakshmi, Ambuj Tripathi, D. K. Avasthi

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Graphene oxide provides a good host matrix for preparing nanocomposites due to the different functional groups attached to its edges and planes. Being biocompatible, it is used in therapeutic applications. As enzyme-based biosensor requires complicated enzyme purification procedure, high fabrication cost and special storage conditions, we need enzyme-less biosensors for use even in a harsh environment like high temperature, varying pH, etc. In this work, we have prepared both enzyme-based and enzyme-less graphene oxide-based biosensors for glucose detection using glucose-oxidase as enzyme and gold nanoparticles, respectively. These samples were characterized using X-ray diffraction, UV-visible spectroscopy, scanning electron microscopy, and transmission electron microscopy to confirm the successful synthesis of the working electrodes. Electrochemical measurements were performed for both the working electrodes using a 3-electrode electrochemical cell. Cyclic voltammetry curves showed the homogeneous transfer of electron on the electrodes in the scan range between -0.2V to 0.6V. The sensing measurements were performed using differential pulse voltammetry for the glucose concentration varying from 0.01 mM to 20 mM, and sensing was improved towards glucose in the presence of gold nanoparticles. Gold nanoparticles in graphene oxide nanocomposite played an important role in sensing glucose in the absence of enzyme, glucose oxidase, as evident from these measurements. The selectivity was tested by measuring the current response of the working electrode towards glucose in the presence of the other common interfering agents like cholesterol, ascorbic acid, citric acid, and urea. The enzyme-less working electrode also showed storage stability for up to 15 weeks, making it a suitable glucose biosensor.

Keywords: electrochemical, enzyme-less, glucose, gold nanoparticles, graphene oxide, nanocomposite

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Authors: R. L. M. Paiva, M. R. Capri, D. R. Mulinari, C. F. Bandeira, S. R. Montoro

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Natural fibers are used in polymer composites to improve mechanical properties, substituting inorganic reinforcing agents produced by non renewable resources. The present study investigates the tensile, flexural and impact behaviors of sugarcane bagasse fibers-polypropylene composite as a function of volume fraction. The surface of the fibers was modified by mercerization treatments to improve the wetting behavior of the apolar polypropylene. The treatment characterization was obtained by infrared spectroscopy and scanning electron microscopy. Results evidence that a good adhesion interfacial between fibers-matrix causing an increase strength and modulus flexural as well as impact strength in the modified fibers/PP composites when compared to the pure PP and unmodified fibers reinforced composites.

Keywords: sugarcane bagasse, polymer composites, mechanical properties, fibers

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Authors: Abderrahmane Hamdi, Julie Chalon, Benoit Dodin, Philippe Champagne

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In this report, we present a simple route to realize robust, hydrophobic, and highly transparent coatings using organic polysilazane (durazane) and zinc oxide nanoparticles (ZnO). These coatings were deposited by spraying the mixture solution on glass slides. Thus, the properties of the films were characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), UV–vis-NIR spectrophotometer, and water contact angle method. This sprayable polymer mixed with ZnO nanoparticles shows high transparency for visible light > 90%, a hydrophobic character (CA > 90°), and good mechanical and chemical stability. The coating also demonstrates excellent self-cleaning properties, which makes it a promising candidate for commercial use.

Keywords: coatings, durability, hydrophobicity, organic polysilazane, self-cleaning, transparence, zinc oxide nanoparticles

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Authors: John Olorunfemi Abe, Olawale Muhammed Popoola, Abimbola Patricia Idowu Popoola

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Hydrogen is an appealing alternative to fossil fuels because of its abundance, low weight, high energy density, and relative lack of contaminants. However, its low density presents a number of storage challenges. Therefore, this work studies the influence of refractory nitride additives consisting of 5 wt. % each of hexagonal boron nitride (h-BN), titanium nitride (TiN), and aluminum nitride (AlN) on hydrogen storage and electrochemical characteristics of Ti6Al4V-based materials produced by spark plasma sintering. The microstructure and phase constituents of the sintered materials were characterized using scanning electron microscopy (in conjunction with energy-dispersive spectroscopy) and X-ray diffraction, respectively. Pressure-composition-temperature (PCT) measurements were used to assess the hydrogen absorption/desorption behavior, kinetics, and storage capacities of the sintered materials, respectively. The pure Ti6Al4V alloy displayed a two-phase (α+β) microstructure, while the modified composites exhibited apparent microstructural modifications with the appearance of nitride-rich secondary phases. It is found that the diffusion process controls the kinetics of the hydrogen absorption. Thus, a faster rate of hydrogen absorption at elevated temperatures ensued. The additives acted as catalysts, lowered the activation energy and accelerated the rate of hydrogen sorption in the composites relative to the monolithic alloy. Ti6Al4V-5 wt. % h-BN appears to be the most promising candidate for hydrogen storage (2.28 wt. %), followed by Ti6Al4V-5 wt. % TiN (2.09 wt. %), whereas Ti6Al4V-5 wt. % AlN shows the least hydrogen storage performance (1.35 wt. %). Accordingly, the developed hydride system (Ti6Al4V-5h-BN) may be competitive for use in applications involving short-range continuous vehicles (~50-100km) as well as stationary applications such as electrochemical devices, large-scale storage cylinders in hydrogen production locations, and hydrogen filling stations.

Keywords: hydrogen storage, Ti6Al4V hydride system, pressure-composition-temperature measurements, refractory nitride additives, spark plasma sintering, Ti6Al4V-based materials

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Authors: Muhammad B. Ibrahim, Muhammad S. Sulaiman, Sadiq Sani

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Neem leaves were studied as plant wastes derived adsorbents for detoxification of Congo Red (CR) and Methyl Orange (MO) from aqueous solutions using batch adsorption technique. The objectives involved determining the effects of the basic adsorption parameters are namely, agitation time, adsorbent dosage, adsorbents particle size, adsorbate loading concentrations and initial pH, on the adsorption process as well as characterizing the adsorbents by determining their physicochemical properties, functional groups responsible for the adsorption process using Fourier Transform Infrared (FTIR) spectroscopy and surface morphology using scanning electron microscopy (SEM) coupled with energy dispersion X – ray spectroscopy (EDS). The adsorption behaviours of the materials were tested against Langmuir, Freundlich, etc. isotherm models. Percent adsorption increased with increase in agitation time (5 – 240 minutes), adsorbent dosage (100-500mg), initial concentration (100-300mg/L), and with decrease in particle size (≥75μm to ≤300μm) of the adsorbents. Both processes are dye pH-dependent, increasing or decreasing percent adsorption in acidic (2-6) or alkaline (8-12) range over the studied pH (2-12) range. From the experimental data the Langmuir’s separation factor (RL) suggests unfavourable adsorption for all processes, Freundlich constant (nF) indicates unfavourable process for CR and MO adsorption; while the mean free energy of adsorption

Keywords: adsorption, congo red, methyl orange, neem leave

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Authors: Alparslan A. Balta, Hilmi Yurdakul, Orkun Tunckan, Servet Turan, Arife Yurdakul

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A silicon oxynitride (Si2N2O), the mineralogical name is “Sinoite”, reveals the outstanding physical, mechanical and thermal properties, e.g., good oxidation resistance at high temperatures, high fracture toughness with rod shape, high hardness, low theoretical density, good thermal shock resistance by low thermal expansion coefficient and high thermal conductivity. In addition, the orthorhombic crystal structure of Si2N2O allows accommodating the rare earth (RE) element atoms along the “c” axis due to existing large structural interstitial sites. Here, 0.02 to 0.12 wt. % Nd3+ doped Si2N2O samples were successfully synthesized by spark plasma sintering (SPS) method at 30MPa pressure and 1650oC temperature. Li2O was also utilized as a sintering additive to take advantage of low eutectic point during synthesizing. The specimens were characterized in detail by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and cathodoluminescence (CL) in SEM and photoluminescence (PL) spectroscopy. Based on the overall results, the Si2N2O phase was obtained above 90% by the SPS route. Furthermore, Nd3+: Si2N2O samples showed a very broad intense emission peak between 400-700 nm, which corresponds to white color. Therefore, this material can be considered as a promising candidate for white light-emitting diodes (WLEDs) purposes. This study was supported by TUBITAK under project number 217M667.

Keywords: neodymium, oxynitride, Si₂N₂O, WLEDs

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Authors: Oyugi Ngure Robert, Kallen Mulilo Nalyanya, Tabitha A. Amollo

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Nanomaterials have attracted significant attention in research because of their exemplary properties, making them suitable for diverse applications. This paper reports the successful synthesis as well as the structural properties of silver sulfide/reduced graphene oxide (Ag_2 S-rGO) nanocomposite. The nanocomposite was synthesized by the chemical reduction method. Scanning electron microscopy (SEM) showed that the reduced graphene oxide (rGO) sheets were intercalated within the Ag_2 S nanoparticles during the chemical reduction process. The SEM images also showed that Ag_2 S had the shape of nanowires. Further, SEM energy dispersive X-ray (SEM EDX) showed that Ag_2 S-rGO is mainly composed of C, Ag, O, and S. X-ray diffraction analysis manifested a high crystallinity for the nanowire-shaped Ag2S nanoparticles with a d-spacing ranging between 1.0 Å and 5.2 Å. Thermal gravimetric analysis (TGA) showed that rGO enhances the thermal stability of the nanocomposite. Ag_2 S-rGO nanocomposite exhibited strong optical absorption in the UV region. The formed nanocomposite is dispersible in polar and non-polar solvents, qualifying it for solution-based device processing.

Keywords: silver sulfide, reduced graphene oxide, nanocomposite, structural properties, optical properties

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Authors: Sheila Shahidi

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UV protection by fabrics has recently become a focus of great interest, particularly in connection with environmental degradation or ozone layer depletion. Fabrics provide simple and convenient protection against UV radiation (UVR), but not all fabrics offer sufficient UV protection. To describe the degree of UVR protection offered by clothing materials, the ultraviolet protection factor (UPF) is commonly used. UV-protective fabric can be generated by application of a chemical finish using normal wet-processing methodologies. However, traditional wet-processing techniques are known to consume large quantities of water and energy and may lead to adverse alterations of the bulk properties of the substrate. Recently, usage of plasmas to generate physicochemical surface modifications of textile substrates has become an intriguing approach to replace or enhance conventional wet-processing techniques. In this research work the effect of plasma treatment on UV protection properties of fabrics was investigated. DC magnetron sputtering was used and the parameters of plasma such as gas type, electrodes, time of exposure, power and, etc. were studied. The morphological and chemical properties of samples were analyzed using Scanning Electron Microscope (SEM) and Furrier Transform Infrared Spectroscopy (FTIR), respectively. The transmittance and UPF values of the original and plasma-treated samples were measured using a Shimadzu UV3101 PC (UV–Vis–NIR scanning spectrophotometer, 190–2, 100 nm range). It was concluded that, plasma which is an echo-friendly, cost effective and dry technique is being used in different branches of the industries, and will conquer textile industry in the near future. Also it is promising method for preparation of UV protection textile.

Keywords: fabric, plasma, textile, UV protection

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Authors: Alain Kusmoko, Druce Dunne, Huijun Li

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Stellite 6 was deposited by laser cladding on a chromium bearing substrate (P91) with energy inputs of 1 kW (P91-1) and 1.8 kW (P91-1.8). The chemical compositions and microstructures of these coatings were characterized by atomic absorption spectroscopy, optical microscopy and scanning electron microscopy. The microhardness of the coatings was measured and the wear mechanism of the coatings was assessed using a pin-on-plate (reciprocating) wear testing machine. The results showed less cracking and pore development for Stellite 6 coatings applied to the P91 steel substrate with the lower heat input (P91-1). Further, the Stellite coating for P91-1 was significantly harder than that obtained for P91-1.8. The wear test results indicated that the weight loss for P91-1 was much lower than for P91-1.8. It is concluded that the lower hardness of the coating for P91-1.8, together with the softer underlying substrate structure, markedly reduced the wear resistance of the Stellite 6 coating.

Keywords: friction and wear, laser cladding, P91 steel, Stellite 6 coating

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Authors: John-Nelson Ekumah, Selorm Yao-Say Solomon Adade, Mingming Zhong, Yufan Sun, Qiufang Liang, Muhammad Safiullah Virk, Xorlali Nunekpeku, Nana Adwoa Nkuma Johnson, Bridget Ama Kwadzokpui, Xiaofeng Ren

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Enhancing starch gel strength and stability is crucial. However, traditional gel property assessment methods are destructive, time-consuming, and resource-intensive. Thus, understanding ethanol treatment effects on kudzu starch gel strength and developing a rapid, nondestructive gel strength assessment method is essential for optimizing the treatment process and ensuring product quality consistency. This study investigated the effects of different ethanol concentrations on the microstructure of kudzu starch gels using a comprehensive microstructural analysis. We also developed a nondestructive method for predicting gel strength and classifying treatment levels using near-infrared (NIR) spectroscopy, and advanced data analytics. Scanning electron microscopy revealed progressive network densification and pore collapse with increasing ethanol concentration, correlating with enhanced mechanical properties. NIR spectroscopy, combined with various variable selection methods (CARS, GA, and UVE) and modeling algorithms (PLS, SVM, and ELM), was employed to develop predictive models for gel strength. The UVE-SVM model demonstrated exceptional performance, with the highest R² values (Rc = 0.9786, Rp = 0.9688) and lowest error rates (RMSEC = 6.1340, RMSEP = 6.0283). Pattern recognition algorithms (PCA, LDA, and KNN) successfully classified gels based on ethanol treatment levels, achieving near-perfect accuracy. This integrated approach provided a multiscale perspective on ethanol-induced starch gel modification, from molecular interactions to macroscopic properties. Our findings demonstrate the potential of NIR spectroscopy, coupled with advanced data analysis, as a powerful tool for rapid, nondestructive quality assessment in starch gel production. This study contributes significantly to the understanding of starch modification processes and opens new avenues for research and industrial applications in food science, pharmaceuticals, and biomaterials.

Keywords: kudzu starch gel, near-infrared spectroscopy, gel strength prediction, support vector machine, pattern recognition algorithms, ethanol treatment

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Authors: Byungsik Moon

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Electron beam inspection (EBI) has played an important role in detecting defects during the Fab process. The study focused on capturing buried Cu metal voids for 5nm technology nodes in Qualcomm Snapdragon mass production. This paper illustrates a case study where Cu metal voids can be detected without side effects with optimized EBI scanning conditions. The voids were buried in the VIA and not detected effectively by bright field inspection. EBI showed higher detectability, about 10 times that of bright fields, and a lower landing energy of EBI can avoid film damage. A comparison of detectability between EBI and bright field inspection was performed, and TEM confirmed voids that were detected by EBI. Therefore, a much higher detectability of buried Cu metal voids can be achieved without causing film damage.

Keywords: electron beam inspection, EBI, landing energy, Cu metal voids, bright field inspection

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Authors: P. Hemalatha, Deepalekshmi Ponnamma, Mariam Al Ali Al-Maadeed

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The Poly(vinylideneflouride-hexafluoropropylene) (PVDF-HFP)/ zinc oxide (ZnO) nanocomposites films were successfully prepared by mixing the fine ZnO particles into PVDF-HFP solution followed by film casting and sandwich techniques. Zinc oxide nanoparticles were synthesized by hydrothermal method. Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to characterize the structure and properties of the obtained nanocomposites. The dielectric properties of the PVDF-HFP/ZnO nanocomposites were analyzed in detail. In comparison with pure PVDF-HFP, the dielectric constant of the nanocomposite (1wt% ZnO) was significantly improved. The piezoelectric co-efficients of the nanocomposites films were measured. Experimental results revealed the influence of filler on the properties of PVDF-HFP and enhancement in the output performance and dielectric properties reflects the ability for energy storage capabilities.

Keywords: dielectric constant, hydrothermal, nanoflowers, organic compounds

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Authors: Asselah Amel, Affif Chaouche M'yassa, Toudji Amira, Tazerouti Amel

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This study covers two aspects ; the biodegradability and the performances in corrosion inhibition of a series of synthetized surfactants namely Φ- sodium methyl ester sulfonates (Φ-MES: C₁₂-MES, C₁₄-MES and C₁₆-MES. The biodegradability of these organic compounds was studied using the respirometric method, ‘the standard ISO 9408’. Degradation was followed by analysis of dissolved oxygen using the dissolved oxygen meter over 28 days and the results were compared with that of sodium dodecyl sulphate (SDS). The inoculum used consists of activated sludge taken from the aeration basin of the biological wastewater treatment plant in the city of Boumerdes-Algeria. In addition, the anticorrosive performances of Φ-MES surfactants on a carbon steel "X70" were evaluated in an injection water from a well of Hassi R'mel region- Algeria, known as Baremian water, and are compared to sodium dodecyl sulphate. Two technics, the weight loss and the linear polarization resistance corrosion rate (LPR) are used allowing to investigate the relationships between the concentrations of these synthetized surfactants and their surface properties, surface coverage and inhibition efficiency. Various adsorption isotherm models were used to characterize the nature of adsorption and explain their mechanism. The results show that the MES anionic surfactants was readily biodegradable, degrading faster than SDS, about 88% for C₁₂-MES compared to 66% for the SDS. The length of their carbon chain affects their biodegradability; the longer the chain, the lower the biodegradability. The inhibition efficiency of these surfactants is around 78.4% for C₁₂-MES, 76.60% for C₁₄-MES and 98.19% for C₁₆-MES and increases with their concentration and reaches a maximum value around their critical micelle concentrations ( CMCs). Scanning electron microscopy coupled to energy dispersive X-ray spectroscopy allowed to the visualization of a good adhesion of the protective film formed by the surfactants to the surface of the steel. The studied surfactants show the Langmuirian behavior from which the thermodynamic parameters as adsorption constant (Kads), standard free energy of adsorption (〖∆G〗_ads^0 ) are determined. Interaction of the surfactants with steel surface have involved physisorptions.

Keywords: corrosion, surfactants, adsorption, adsorption isotherems

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Authors: Pham-Thi Huong, Byeong-Kyu Lee, Jitae Kim, Chi-Hyeon Lee

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Fe-nano zeolite adsorbent was used for removal of Ni (II) ions from aqueous solution. The adsorbent was characterized by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and the surface area Brunauer–Emmett–Teller (BET) using for analysis of functional groups, morphology and surface area. Bath adsorption experiments were analyzed on the effect of pH, time, adsorbent doses and initial Ni (II) concentration. The optimum pH for Ni (II) removal using Fe-nano zeolite was found at 5.0 and 90 min of reaction time. The maximum adsorption capacity of Ni (II) was 231.68 mg/g based on the Langmuir isotherm. The kinetics data for the adsorption process was fitted with the pseudo-second-order model. The desorption of Ni (II) from Ni-loaded Fe-nano zeolite was analyzed and even after 10 cycles 72 % desorption was achieved. These finding supported that Fe-nano zeolite with high adsorption capacity, high reuse ability would be utilized for Ni (II) removal from water.

Keywords: Fe-nano zeolite, adsorption, Ni (II) removal, regeneration

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Authors: Nyiko M. Chauke, James Ramontja, Richard M. Moutloali

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The zeolite ZSM-22 material demonstrated effective hydrophilic character as a nanoadditive filler in the preparation of nanocomposite membranes. In this study, nanorods ZSM-22 zeolite materials were hydrothermally synthesised from a homogenous gel mixture prepared using different silica precursors: colloidal silica, fumed silica, tetraethylorthosilicate (TEOS), and aluminium precursor: aluminium sulphate octadecahydrate (Al₂(SO₄)₃.18H₂O to Si/Al of 60. This was focused on developing a defect-free zeolite framework for effective use in applications such as membrane separation process, adsorption, and catalysis. The obtained ZSM-22 zeolite materials with 60 Si/Al ratio exhibits high crystallinity, hydrophilicity, and needle-like morphologies, suggesting successful synthesis as shown by X-ray Diffraction (XRD), Brunauer-Emmett-Teller (BET), Fourier-Transform Infrared Spectroscopy (FTIR), Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM) physicochemical analysis. It was revealed that the use of different nature of silica precursors significantly influenced the properties of the final product and contributed to the development of defect-free zeolite material. As such, the crystalline nanorods of Theta-1 (TON) ZSM-22 obtained from TEOS silica showed high phase purity, defect-free, and narrow particle size distribution. Morphological analysis exhibited that the use of TEOS as silica precursor was effective than its counterparts and produced high crystalline need-like agglomerated particles.

Keywords: silica precursor, hydrothermal synthesis, zeolite material, ZSM-22

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Authors: Shadatul Hanom Rashid, Xiaorong Zhou

Abstract:

Hybrid sol-gel coatings are the blend of both advantages of inorganic and organic networks have been reported as environmentally friendly anti-corrosion surface pre-treatment for several metals, including aluminum alloys. In this current study, Si-Zr hybrid sol-gel coatings were synthesized from (3-glycidoxypropyl)trimethoxysilane (GPTMS), tetraethyl orthosilicate (TEOS) and zirconium(IV) propoxide (TPOZ) precursors and applied on AA6111 aluminum alloy by dip coating technique. The hybrid sol-gel coatings doped with different concentrations of cerium nitrate (Ce(NO3)3) as a corrosion inhibitor were also prepared and the effect of Ce(NO3)3 concentrations on the morphology and corrosion resistance of the coatings were examined. The surface chemistry and morphology of the hybrid sol-gel coatings were analyzed by Fourier transform infrared (FTIR) spectroscopy and scanning electron microscopy (SEM). The corrosion behavior of the coated aluminum alloy samples was evaluated by electrochemical impedance spectroscopy (EIS). Results revealed that good corrosion resistance of hybrid sol-gel coatings were prepared from hydrolysis and condensation reactions of GPTMS, TEOS and TPOZ precursors deposited on AA6111 aluminum alloy. When the coating doped with cerium nitrate, the properties were improved significantly. The hybrid sol-gel coatings containing lower concentration of cerium nitrate offer the best inhibition performance. A proper doping concentration of Ce(NO3)3 can effectively improve the corrosion resistance of the alloy, while an excessive concentration of Ce(NO3)3 would reduce the corrosion protection properties, which is associated with defective morphology and instability of the sol-gel coatings.

Keywords: AA6111, Ce(NO3)3, corrosion, hybrid sol-gel coatings

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Authors: Abdullah Faqihi, John Hedley

Abstract:

Biosensors play a significant role in the healthcare sectors, scientific and technological progress. Developing electrodes that are easy to manufacture and deliver better electrochemical performance is advantageous for diagnostics and biosensing. They can be implemented extensively in various analytical tasks such as drug discovery, food safety, medical diagnostics, process controls, security and defence, in addition to environmental monitoring. Development of biosensors aims to create high-performance electrochemical electrodes for diagnostics and biosensing. A biosensor is a device that inspects the biological and chemical reactions generated by the biological sample. A biosensor carries out biological detection via a linked transducer and transmits the biological response into an electrical signal; stability, selectivity, and sensitivity are the dynamic and static characteristics that affect and dictate the quality and performance of biosensors. In this research, a developed experimental study for laser scribing technique for graphene oxide inside a vacuum chamber for processing of graphene oxide is presented. The processing of graphene oxide (GO) was achieved using the laser scribing technique. The effect of the laser scribing on the reduction of GO was investigated under two conditions: atmosphere and vacuum. GO solvent was coated onto a LightScribe DVD. The laser scribing technique was applied to reduce GO layers to generate rGO. The micro-details for the morphological structures of rGO and GO were visualised using scanning electron microscopy (SEM) and Raman spectroscopy so that they could be examined. The first electrode was a traditional graphene-based electrode model, made under normal atmospheric conditions, whereas the second model was a developed graphene electrode fabricated under a vacuum state using a vacuum chamber. The purpose was to control the vacuum conditions, such as the air pressure and the temperature during the fabrication process. The parameters to be assessed include the layer thickness and the continuous environment. Results presented show high accuracy and repeatability achieving low cost productivity.

Keywords: laser scribing, lightscribe DVD, graphene oxide, scanning electron microscopy

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Authors: K. Abbas, R. Ahmad, I. A. Khan, S. Saleem, U. Ikhlaq

Abstract:

Nitriding of p-type Si samples by pulsed DC glow discharge is carried out for different Ar concentrations (30% to 90%) in nitrogen-argon plasma whereas the other parameters like pressure (2 mbar), treatment time (4 hr) and power (175 W) are kept constant. The phase identification, crystal structure, crystallinity, chemical composition, surface morphology and topography of the nitrided layer are studied using X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FTIR), optical microscopy (OM), scanning electron microscopy (SEM) and atomic force microscopy (AFM) respectively. The XRD patterns reveal the development of different diffraction planes of Si₃N₄ confirming the formation of polycrystalline layer. FTIR spectrum confirms the formation of bond between Si and N. Results reveal that addition of Ar into N₂ plasma plays an important role to enhance the production of active species which facilitate the nitrogen diffusion.

Keywords: crystallinity, glow discharge, nitriding, sputtering

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Authors: R. S. Yadav, J. Havlica, I. Kuřitka, Z. Kozakova, J. Masilko, M. Hajdúchová, V. Enev, J. Wasserbauer

Abstract:

In this present work, CoFe2-xNdxO4 (0.0 ≤ x ≥0.1) spinel ferrite nanoparticles were synthesized by starch-assisted sol-gel auto-combustion method. Powder X-ray diffraction patterns were revealed the formation of cubic spinel ferrite with the signature of NdFeO3 phase at higher Nd3+ concentration. The field emission scanning electron microscopy study demonstrated the spherical nanoparticle in the size range between 5-15 nm. Raman and Fourier Transform Infrared spectra supported the formation of the spinel ferrite structure in the nanocrystalline form. The X-ray photoelectron spectroscopy (XPS) analysis confirmed the presence of Co2+ and Fe3+ at octahedral as well as a tetrahedral site in CoFe2-xNdxO4 nanoparticles. The change in magnetic properties with a variation of concentration of Nd3+ ions in cobalt ferrite nanoparticles was observed.

Keywords: nanoparticles, spinel ferrites, sol-gel auto-combustion method, CoFe2-xNdxO4

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Authors: Rasim Alguliev, Farhad Yusifov

Abstract:

Considering the international experience, conceptual and architectural principles of forming of electron government are researched and some suggestions were made. The assessment of monitoring of forming processes of electron government, intellectual analysis of web-resources, provision of information security, electron democracy problems were researched, conceptual approaches were suggested. By taking into consideration main principles of electron government theory, important research directions were specified.

Keywords: electron government, public administration, information security, web-analytics, social networks, data mining

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Authors: Mechri hanane, Azzaz Mohammed

Abstract:

Polycrystalline CuFe thin film was prepared by thermal evaporation process (Physical vapor deposition), using the nanocrystalline CuFe powder obtained by mechanical alloying After 24 h of milling elemental powders. The microscopic study of nanocrystalline powder and the thin film of Cu70Fe30 binary alloy were examined using transmission electron microscopy (TEM) and scanning electron microscope (SEM). The cross-sectional TEM images showed that the obtained CuFe layer was polycrystalline film of about 20 nm thick and composed of grains of different size ranging from 4 nm to 18 nm.

Keywords: nanomaterials, thin films, TEM, SEM

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Authors: S. Raeis Farshid, B. Raeis Farshid

Abstract:

Ag-TiO₂ nanocomposites were prepared by the sol-gel method with and without additives such as carboxy methyl cellulose (CMC), polyethylene glycol (PEG), polyvinyl pyrrolidone (PVP), and hydroxyl propyl cellulose (HPC). The characteristics of the prepared Ag-TiO₂ nanocomposites were identified by Fourier Transform Infra-Red spectroscopy (FTIR), X-Ray Diffraction (XRD), and scanning electron microscopy (SEM) methods. The additives have a significant effect on the particle size distribution and photocatalytic activity of Ag-TiO₂ nanocomposites. SEM images have shown that the particle size distribution of Ag-TiO₂ nanocomposite in the presence of HPC was the best in comparison to the other samples. The photocatalytic activity of the synthesized nanocomposites was investigated for decolorization of methyl orange (MO) in water under UV-irradiation in a batch reactor, and the results showed that the photocatalytic activity of the nanocomposites had been increased by CMC, PEG, PVP, and HPC, respectively.

Keywords: sol-gel method, Ag-TiO₂, decolorization, photocatalyst, nanocomposite

Procedia PDF Downloads 80