Search results for: confocal microscopy

Authors: Charles Klein O. Gorit, Mark Tristan J. Quimque Jr., M. Cecilia V. Almeda, Concepcion M. Salvana

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Chitosan is a promising biopolymer commonly found in crustacean shells that has plausible effects in water purification and wastewater treatment. It is a primary derivative of chitin and considered second of the most abundant biopolymer prior to cellulose. Morphological analysis had been done using Scanning Electron Microscopy with Energy Dispersive Microscopy (SEM/EDS), and due to its porous nature, it showcases a certain degree of porosity, hence, larger adsorption site of heavy metal. The Energy Dispersive Spectroscopy of the chitosan and ‘lead-bound’ chitosan, shows a relative increase of percent abundance of lead cation from 1.44% to 2.08% hence, adsorption occurs. Chitosan, as a nitrogenous polysaccharide, subjected to Fourier transform infrared spectroscopy (FTIR) analysis shows amide bands ranging from 1635.36 cm⁻¹ for amide 1 band and 1558.40 cm-1 for amide 2 band with NH stretching. For ‘lead-bound’ chitosan, the FT-IR analysis shows a change in peaks upon adsorption of Pb(II) cation. The spectrum shows broadening of OH and NH stretching band. Such observation can be attributed to the probability that the attachment of Pb(II) ions is in these functional groups. A column filter was devised with lead-bound chitosan to determine the zero point charge (pHzpc) of the biopolymer. The results show that at pH 8.34, below than the zpc level of literatures cited for lead which ranges from pH 4 to 7, favors the adsorption site of chitosan and its capability to adsorb traces amount of aqueous lead.

Keywords: chitosan, biopolymer, FT-IR, SEM, zero-point charge, heavy metal, lead ions

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Authors: Nicoleta Simona Vedeanu, Rares Stiufiuc, Dana Alina Magdas

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A detailed knowledge of the teeth structure is mandatory to understand and explain the defects and the dental pathology, but especially to take a correct decision regarding dental prophylaxis and treatment. The present work is an alternative study to the traditional investigation methods used in dentistry, a study based on the use of modern, sensitive physical methods to investigate human enamel and dentin. For the present study, several teeth collected from patients of different ages were used for structural and dietary investigation. The samples were investigated by Raman spectroscopy for the molecular structure analysis of dentin and enamel, atomic force microscopy (AFM) to view the dental topography at the micrometric size and mass spectrometry for isotopic ratios as a fingerprint of patients’ personal diet. The obtained Raman spectra and their interpretation are in good correlation with the literature and may give medical information by comparing affected dental structures with healthy ones. AFM technique gave us the possibility to study in details the dentin and enamel surface to collect information about dental hardness or dental structural changes. δ¹³C values obtained for the studied samples can be classified in C4 category specific to young people and children diet (sweets, cereals, juices, pastry). The methods used in this attempt furnished important information about dentin and enamel structure and dietary habits and each of the three proposed methods can be extended at a larger level in the study of the teeth structure.

Keywords: AFM, dentine, enamel, Raman spectroscopy

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Authors: Keivan Jamshidi

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Distal swelling and eventual degeneration of axon in the CNS and PNS have been considered to be the characteristic neuropathological effects of acrylamide (ACR) neuropathy. This study was conducted to determine the neurotoxic effects of different doses of ACR (0.5, 5, 50, 100, and 500 mg/kg per day × 11days i. p.) on hypothalamus of rat using the de Olmos amino cupric-silver stain and electron microscopy. For this purpose 60 adult male rats (Wistar, approximately 250 g) were randomly assigned in 5 treatment groups as A, B, C, D, E) exposed to 0.5, 5, 50, 100, and 500 mg/kg per dayx11days i. p. and one control group as F received daily i. p. injections of 0.9% saline (3ml/kg). As indices of developing neurotoxicity, weight gain, gait scores and landing hindlimb foot splay were determined. After 11 days, two rats for silver stain, and two rats for EM were randomly selected; dissected and proper samples were collected from hypothalamus. Results did show no neurological behavior in groups A, B and F were observed in group C. Rats in groups D and E died within 1-2 hours due to sever toxemia. In histopathological studies based on de Olmos technique no argyrophilic neurons or processes were observed in stained sections obtained from hypothalamus of rats belong to groups A, B, and F while moderate to severe argyrophilic changes were observed in different nuclei and regions of stained sections obtained from hypothalamus of rats belong to group C. In ultra-structural studies some variations in the myelin sheet of injured axons including decompactation, interlaminar space formation, disruption of the laminar sheet, accumulation of neurofilaments, vacculation, and clumping inside the axolem, and finally complete disappearance of laminar sheet were observed.

Keywords: acrylamide, hypothalamus, rat, de Olmos amino cupric, silver stain, electron microscopy

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Authors: Yuliya Huseva

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To investigate the contents of tears to determine latent blood. Methods: Tear samples from 72 women were studied with the microscopy of tears aspirated with a capillary and stained by Nocht and with a chemical method of test strips with chromogen. Statistical data processing was carried out using statistical packages Statistica 10.0 for Windows, calculation of Pearson's chi-square test, Yule association coefficient, the method of determining sensitivity and specificity. Results:, In 30.6% (22) of tear samples erythrocytes were revealed microscopically. Correlations between the presence of erythrocytes in the tear and the phase of the menstrual cycle has been discovered. In the follicular phase of the cycle, erythrocytes were found in 59.1% (13) people, which is significantly more (x2=4.2, p=0.041) compared to the luteal phase - in 40.9% (9) women. In the first seven days of the follicular phase of the menstrual cycle the erythrocytes were predominanted of in the tears of women examined testifies in favour of the vicarious bleeding from the mucous membranes of extragenital organs in sync with menstruation. Of the other cellular elements in tear samples with latent haemolacria, neutrophils prevailed - in 45.5% (10), while lymphocytes were less common - in 27.3% (6), because neutrophil exudation is accompanied by vasodilatation of the conjunctiva and the release of erythrocytes into the conjunctival cavity. It was found that the prognostic significance of the chemical method was 0.53 of the microscopic method. In contrast to microscopy, which detected blood in tear samples from 30.6% (22) of women, blood was detected chemically in tears of 16.7% (12). An association between latent haemolacria and endometriosis was found (k=0.75, p≤0.05). Microscopically, in the tears of patients with endometriosis, erythrocytes were detected in 70% of cases, while in healthy women without endometriosis - in 25% of cases. The proportion of women with erythrocytes in tears, determined by a chemical method, was 41.7% among patients with endometriosis, which is significantly more (x2=6.5, p=0.011) than 11.7% among women without endometriosis. The data obtained can be explained by the etiopathogenesis of the extragenital endometriosis which is caused by hematogenous spread of endometrial tissue into the orbit. In endometriosis, erythrocytes are found against the background of accumulations of epithelial cells. In the tear samples of 4 women with endometriosis, glandular cuboidal epithelial cells, morphologically similar to endometrial cells, were found, which may indicate a generalization of the disease. Conclusions: Single erythrocytes can normally be found in the tears, their number depends on the phase of the menstrual cycle, increasing in the follicular phase. Erythrocytes found in tears against the background of accumulations of epitheliocytes and their glandular atypia may indicate a manifestation of extragenital endometriosis. Both used methods (microscopic and chemical) are informative in revealing latent haemolacria. The microscopic method is more sensitive, reveals intact erythrocytes, and besides, it provides information about other cells. At the same time, the chemical method is faster and technically simpler, it determines the presence of haemoglobin and its metabolic products, and can be used as a screening.

Keywords: tear, blood, microscopy, epitheliocytes

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Authors: Abhimanyu Thakur, Youngjin Lee

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Glioma is a lethal brain cancer whose early diagnosis and prognosis are limited due to the dearth of a suitable technique for its early detection. Current approaches, including magnetic resonance imaging (MRI), computed tomography (CT), and invasive biopsy for the diagnosis of this lethal disease, hold several limitations, demanding an alternative method. Recently, extracellular vesicles (EVs) have been used in numerous biomarker studies, majorly exosomes and microvesicles (MVs), which are found in most of the cells and biofluids, including blood, cerebrospinal fluid (CSF), and urine. Remarkably, glioma cells (GMs) release a high number of EVs, which are found to cross the blood-brain-barrier (BBB) and impersonate the constituents of parent GMs including protein, and lncRNA; however, biophysical properties of EVs have not been explored yet as a biomarker for glioma. We isolated EVs from cell culture conditioned medium of GMs and regular primary culture, blood, and urine of wild-type (WT)- and glioma mouse models, and characterized by nano tracking analyzer, transmission electron microscopy, immunogold-EM, and differential light scanning. Next, we measured the biophysical parameters of GMs-EVs by using atomic force microscopy. Further, the functional constituents of EVs were examined by FTIR and Raman spectroscopy. Exosomes and MVs-derived from GMs, blood, and urine showed distinction biophysical parameters (roughness, adhesion force, and stiffness) and different from that of regular primary glial cells, WT-blood, and -urine, which can be attributed to the characteristic functional constituents. Therefore, biophysical features can be potential diagnostic biomarkers for glioma.

Keywords: glioma, extracellular vesicles, exosomes, microvesicles, biophysical properties

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Authors: Ananya Barui, Provas Banerjee, Jyotirmoy Chatterjee

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Application of optical technology in medicine and biology has a long track-record. In this endeavor, OCT is able to attract both engineers and biologists to work together in the field of photonics for establishing a striking non-invasive imaging technology. In contrast to other in vivo imaging modalities like Raman imaging, confocal imaging, two-photon microscopy etc. which can perform in vivo imaging upto 100-200 micron depth due to limitation in numerical aperture or scattering, however, OCT can achieve high-resolution imaging upto few millimeters of tissue structures depending on their refractive index in different anatomical location. This tomographic system depends on interference of two light waves in an interferometer to produce a depth profile of specimen. In wound healing, frequent collection of biopsies for follow-up of repair process could be avoided by such imaging technique. Real time skin OCT (the optical biopsy) has efficacy in deeper and faster illumination of cutaneou tissue to acquire high resolution cross sectional images of their internal micro-structure. Swept Source-OCT (SS-OCT), a novel imaging technique, can generate high-speed depth profile (~ 2 mm) of wound at a sweeping rate of laser with micron level resolution and optimum coherent length of 5-6 mm. Normally multi-layered skin tissue depicts different optical properties along with variation in thickness, refractive index and composition (i.e. keratine layer, water, fat etc.) according to their anatomical location. For instance, stratum corneum, the upper-most and relatively dehydrated layer of epidermis reflects more light and produces more lucid and a sharp demarcation line with rest of the hydrated epidermal region. During wound healing or regeneration, optical properties of cutaneous tissue continuously altered with maturation of wound bed. More mature and less hydrated tissue component reflects more light and becomes visible as a brighter area in comparison to immature region which content higher amount water or fat that depicts as a darker area in OCT image. Non-healing wound possess prolonged inflammation and inhibits nascent proliferative stage. Accumulation of necrotic tissues also prevents the repair of non-healing wounds. Due to high resolution and potentiality to reflect the compositional aspects of tissues in terms of their optical properties, this tomographic method may facilitate in differentiating non-healing and acute wounds in addition to clinical observations. Non-invasive OCT offers better insight regarding specific biological status of tissue in health and pathological conditions, OCT images could be associated with histo-pathological ‘gold standard’. This correlated SS-OCT and microscopic evaluation of the wound edges can provide information regarding progressive healing and maturation of the epithelial components. In the context of searching analogy between two different imaging modalities, their relative performances in imaging of healing bed were estimated for probing an alternative approach. Present study validated utility of SS-OCT in revealing micro-anatomic structure in the healing bed with newer information. Exploring precise correspondence of OCT images features with histo-chemical findings related to epithelial integrity of the regenerated tissue could have great implication. It could establish the ‘optical biopsy’ as a potent non-invasive diagnostic tool for cutaneous pathology.

Keywords: histo-pathology, non invasive imaging, OCT, wound healing

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Authors: Ram Mohan, Mahendran Samykano, Shyam Aravamudhan

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Metallic nanowires with sub-micron and hundreds of nanometer diameter have a diversity of applications in nano/micro-electromechanical systems (NEMS/MEMS). Characterizing the mechanical properties of such sub-micron and nano-scale metallic nanowires are tedious; require sophisticated and careful experimentation to be performed within high-powered microscopy systems (scanning electron microscope (SEM), atomic force microscope (AFM)). Also, needed are nanoscale devices for placing the nanowires; loading them with the intended conditions; obtaining the data for load–deflection during the deformation within the high-powered microscopy environment poses significant challenges. Even picking the grown nanowires and placing them correctly within a nanoscale loading device is not an easy task. Mechanical characterizations through experimental methods for such nanowires are still very limited. Various techniques at different levels of fidelity, resolution, and induced errors have been attempted by material science and nanomaterial researchers. The methods for determining the load, deflection within the nanoscale devices also pose a significant problem. The state of the art is thus still at its infancy. All these factors result and is seen in the wide differences in the characterization curves and the reported properties in the current literature. In this paper, we discuss and present our experimental method, results, and discussions of uniaxial tensile loading and the development of subsequent stress–strain characteristics curves for Nickel nanowires. Nickel nanowires in the diameter range of 220–270 nm were obtained in our laboratory via an electrodeposition method, which is a solution based, template method followed in our present work for growing 1-D Nickel nanowires. Process variables such as the presence of magnetic field, its intensity; and varying electrical current density during the electrodeposition process were found to influence the morphological and physical characteristics including crystal orientation, size of the grown nanowires1. To further understand the correlation and influence of electrodeposition process variables, associated formed structural features of our grown Nickel nanowires to their mechanical properties, careful experiments within scanning electron microscope (SEM) were conducted. Details of the uniaxial tensile characterization, testing methodology, nanoscale testing device, load–deflection characteristics, microscopy images of failure progression, and the subsequent stress–strain curves are discussed and presented.

Keywords: uniaxial tensile characterization, nanowires, electrodeposition, stress-strain, nickel

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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: G. Karunakaran, M. Jagathambal, N. Van Minh, E. Kolesnikov, A. Gusev, O. V. Zakharova, E. V. Scripnikova, E. D. Vishnyakova, D. Kuznetsov

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Iron oxide nanoparticles (Fe₂O₃NPs) are widely used in different applications due to its ecofriendly nature and biocompatibility. Hence, in this investigation, biosynthesized Fe₂O₃NPs influence on flax (Linum usitatissimum L.) plant was examined. The biosynthesized nanoparticles were found to be cubic phase which is confirmed by XRD analysis. FTIR analysis confirmed the presence of functional groups corresponding to the iron oxide nanoparticle. The elemental analysis also confirmed that the obtained nanoparticle is iron oxide nanoparticle. The scanning electron microscopy and the transmission electron microscopy confirm that the average particle size was around 56 nm. The effect of Fe₂O₃NPs on seed germination followed by biochemical analysis was carried out using standard methods. The results obtained after four days and 11 days of seed vigor studies showed that the seedling length (cm), average number of seedling with leaves, increase in root length (cm) was found to be enhanced on treatment with iron oxide nanoparticles when compared to control. A positive correlation was noticed with the dose of the nanoparticle and plant growth, which may be due to changes in metabolic activity. Hence, to evaluate the change in metabolic activity, peroxidase and catalase activities were estimated. It was clear from the observation that higher concentration of iron oxide nanoparticles (Fe₂O₃NPs 1000 mg/L) has enhanced peroxidase and catalase activities and in turn plant growth. Thus, this study clearly showed that biosynthesized iron oxide nanoparticles will be an effective nano-nutrient for agriculture applications.

Keywords: catalase, fertilizer, iron oxide nanoparticles, Linum usitatissimum L., nano-nutrient, peroxidase

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Authors: Nazanin Sheibanian, Raffaella Sesana, Sedat Ozbilen

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In recent years, high-entropy alloys (HEAs) have attracted considerable attention due to their unique properties and potential applications. In this study, novel HEA coatings were prepared on Mg substrates using mechanically alloyed HEA powder feedstocks based on Al_(0.1-0.5)CoCrCuFeNi and MnCoCrCuFeNi multi-material systems. The coatings were deposited by the Cold Spray (CS) process using three different temperatures of the process gas (N2) (650°C, 750°C, and 850°C) to examine the effect of gas temperature on coating properties. In this study, Infrared Thermography (non-destructive) was examined as a possible quality control technique for HEA coatings applied to magnesium substrates. Active Thermography was employed to characterize coating properties using the thermal response of the coating. Various HEA chemical compositions and deposition temperatures have been investigated. As a part of this study, a comprehensive macro and microstructural analysis of Cold Spray (CS) HEA coatings has been conducted using macrophotography, optical microscopy, scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM+EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), microhardness tests, roughness measurements, and porosity assessments. These analyses provided insight into phase identification, microstructure characterization, deposition, particle deformation behavior, bonding mechanisms, and identifying a possible relationship between physical properties and thermal responses. Based on the figures and tables, it is evident that the Maximum Relative Radiance (∆RMax) of each sample differs depending on both the chemical composition of HEA and the temperature at which Cold Spray is applied.

Keywords: active thermography, coating, cold spray, high- entropy alloy, material characterization

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Authors: Mudawi M. Nour

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Background: Now a days, the multidisciplinary scientific research conception in the field of nanotechnology has witnessed development with regard to the numerous applications and synthesis of nanomaterials. Objective: The current investigation has been conducted with the main focus on the green synthesis of silver nanoparticles from the leaves of Salvadora persica and its antibacterial activity against MDR pathogens E. coli and S. aureus. Methodology: Silver nanoparticles (AgNPs) were prepared after addition of aqueous extract of Salvadora persica leaves. The UV-Vis spectrophotometer, Transmission Electron Microscopy (TEM), zeta potential and Scanning Electron Microscopy (SEM) were employed to detect the particle size and morphology, besides Fourier transform infra-red spectrometer (FTIR) analysis was performed to determine the capping and stabilizing agents in the extract. Antibacterial assay for the biogenic AgNPs was conducted against E. coli and S. aureus. Results: Color change of the mixture from yellow to dark brown is the first indication to AgNPs formation. Furthermore, 420 nm was the peak value for UV-Vis spectroscopy absorption of the mixture. Besides, TEM and SEM micrographs showed wide variability in the diameter of smaller NPs aggregated together with spherical shapes, and zeta sizer showed about 153.3 nm as an average size of nanoparticles. Microbial suppression was noticed for the tested microorganisms. Furthermore, with the help of FTIR analysis, the biomolecules that act as capping and stabilizing agents of AgNPs are proteins and phenols present in the plant extract. Conclusion: Salvadora persica leaves extract act as a reducing and stabilizing agent for the synthesis of AgNPs, keeping its ability to suppress the MDR pathogen.

Keywords: green synthesis, FTIR, MDR pathogen, salvadora persica

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Authors: Raj Kumar, Prem Felix Siril

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The poor aqueous solubility of many pharmaceutical drugs and potential drug candidates is a big challenge in drug development. Nanoformulation of such candidates is one of the major solutions for the delivery of such drugs. We initially developed the evaporation assisted solvent-antisolvent interaction (EASAI) method. EASAI method is use full to prepared nanoparticles of poor water soluble drugs with spherical morphology and particles size below 100 nm. However, to further improve the effect formulation to reduce number of dose and side effect it is important to control the delivery of drugs. However, many drug delivery systems are available. Among the many nano-drug carrier systems, solid lipid nanoparticles (SLNs) have many advantages over the others such as high biocompatibility, stability, non-toxicity and ability to achieve controlled release of drugs and drug targeting. SLNs can be administered through all existing routes due to high biocompatibility of lipids. SLNs are usually composed of lipid, surfactant and drug were encapsulated in lipid matrix. A number of non-steroidal anti-inflammatory drugs (NSAIDs) have poor bioavailability resulting from their poor aqueous solubility. In the present work, SLNs loaded with NSAIDs such as Nabumetone (NBT), Ketoprofen (KP) and Ibuprofen (IBP) were successfully prepared using different lipids and surfactants. We studied and optimized experimental parameters using a number of lipids, surfactants and NSAIDs. The effect of different experimental parameters such as lipid to surfactant ratio, volume of water, temperature, drug concentration and sonication time on the particles size of SLNs during the preparation using hot-melt sonication was studied. It was found that particles size was directly proportional to drug concentration and inversely proportional to surfactant concentration, volume of water added and temperature of water. SLNs prepared at optimized condition were characterized thoroughly by using different techniques such as dynamic light scattering (DLS), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), X-ray diffraction (XRD) and differential scanning calorimetry and Fourier transform infrared spectroscopy (FTIR). We successfully prepared the SLN of below 220 nm using different lipids and surfactants combination. The drugs KP, NBT and IBP showed 74%, 69% and 53% percentage of entrapment efficiency with drug loading of 2%, 7% and 6% respectively in SLNs of Campul GMS 50K and Gelucire 50/13. In-vitro drug release profile of drug loaded SLNs is shown that nearly 100% of drug was release in 6 h.

Keywords: nanoparticles, delivery, solid lipid nanoparticles, hot-melt sonication, poor water soluble drugs, solubility, bioavailability

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Authors: Amal A. Al-Kahlawy, Heba H. El-Maghrabi

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Due to the increasing need to environment protection in real time need to energize new materials are under extensive investigations. Between others, TiO2 nanotubes (TNTs) nanocomposite with iron oxide and silver carbonate, are promising alternatives as high-efficiency visible light photocatalyst due to their unique properties and their superior charge transport properties. Our efforts in this domain aim the construction of novel nanocomposite of TiO2NT/Fe2O3@Ag2CO3. The structure, surface morphology, chemical composition and optical properties were characterized by X-ray diffraction (XRD), Raman, Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDS), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and UV–vis diffuse reflectance spectroscopy (DRS). XRD results confirm the interaction of TiO2-NT with iron oxide. This novel nanocomposite shows remarkably enhanced performance for phenol compounds photodegradation. The experimental data shows a promising photocatalytic activity. In particular, a maximum value of 450 mg/g was removed within 60 min at solar light irradiation with degradation efficiency of 99.5%. The high photocatalytic activity of the nanocomposite is found to be related to the increased adsorption toward chemical species, enhanced light absorption and efficient charge separation and transfer. Finally, the designed TiO2NT/Fe2O3@Ag2CO3 nanocomposite has a great degree of sustainability and could has a potential application for the industrial treatment of wastewater containing toxic organic materials.

Keywords: nanocomposite, photocatalyst, solar energy, titanium dioxide nanotubes

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Authors: Omar Concepcion, Osvaldo De Melo, Arturo Escobosa

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Topological insulator (TI) materials are insulating in the bulk and conducting in the surface. The unique electronic properties associated with these surface states make them strong candidates for exploring innovative quantum phenomena and as practical applications for quantum computing, spintronic and nanodevices. Many materials, including Bi₂Te₃, have been proposed as TIs and, in some cases, it has been demonstrated experimentally by angle-resolved photoemission spectroscopy (ARPES), scanning tunneling spectroscopy (STM) and/or magnetotransport measurements. A clean surface is necessary in order to make any of this measurements. Several techniques have been used to produce films and different kinds of nanostructures. Growth and characterization in situ is usually the best option although cleaving the films can be an alternative to have a suitable surface. In the present work, we report a comparison of Bi₂Te₃ grown by physical vapor transport (PVT) and molecular beam epitaxy (MBE). The samples were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and ARPES. The Bi₂Te₃ samples grown by PVT, were cleaved in the ultra-high vacuum in order to obtain a surface free of contaminants. In both cases, the XRD shows a c-axis orientation and the pole diagrams proved the epitaxial relationship between film and substrate. The ARPES image shows the linear dispersion characteristic of the surface states of the TI materials. The samples grown by PVT, a relatively simple and cost-effective technique shows the same high quality and TI properties than the grown by MBE.

Keywords: Bismuth telluride, molecular beam epitaxy, physical vapor transport, topological insulator

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Authors: Carmen M. Gonzalez-Henriquez, Mauricio A. Sarabia-Vallejos, Juan Rodriguez-Hernandez

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DMAEMA, as a monomer, has been widely studied and used in several application fields due to their pH-sensitive capacity (tertiary amine protonation), being relevant in the biomedical area as a potential carrier for drugs focused on the treatment of genetic or acquired diseases (efficient gene transfection), among others. Additionally, the inhibition of bacterial growth and, therefore, their antimicrobial activity, can be used as dual-functional antifogging/antimicrobial polymer coatings. According to their interesting physicochemical characteristics and biocompatible properties, DMAEMA was used as a monomer to synthesize a smart pH-sensitive hydrogel, namely poly(HEMA-co-PEGDA575-co-DMAEMA). Thus, different mole ratios (ranging from 5:1:0 to 0:1:5, according to the mole ratio between HEMA, PEGDA, and DEAEMA, respectively) were used in this research. The surface patterns formed via a two-step polymerization (redox- and photo-polymerization) were first chemically studied via 1H-NMR and elemental analysis. Secondly, the samples were morphologically analyzed by using Field-Emission Scanning Electron Microscopy (FE-SEM) and Atomic Force Microscopy (AFM) techniques. Then, a particular relation between HEMA, PEGDA, and DEAEMA (0:1:5) was also characterized at three different pH (5.4, 7.4 and 8.3). The hydrodynamic radius and zeta potential of the micro-hydrogel particles (emulsion) were carried out as a possible control for morphology, exploring the effect that produces hydrogel micelle dimensions in the wavelength, height, and roughness of the wrinkled patterns. Finally, contact angle and cross-hatch adhesion test was carried out for the hydrogels supported on glass using TSM-silanized surfaces in order to measure their mechanical properties.

Keywords: wrinkled patterns, smart pH-sensitive hydrogels, hydrogel micelle diameter, adhesion tests

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Authors: Hadjer Didouh, Izzaddine Sameut Bouhaik, Mohammed Hadj Meliani

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This research delves into the intricate dynamics of biofilm adhesion on surfaces, particularly focusing on the widely employed X52 surface in oil and gas industry pipelines. Biofilms, characterized by microorganisms within a self-produced matrix, pose significant challenges due to their detrimental impact on surfaces. Our study integrates advanced molecular techniques and cutting-edge microscopy, such as scanning electron microscopy (SEM), to identify microbial communities and visually assess biofilm adhesion. Simultaneously, we concentrate on the X52 surface, utilizing impedance spectroscopy and potentiodynamic polarization to gather electrochemical responses under various conditions. In conjunction with the broader investigation, we propose a novel approach to mitigate biofilm-induced corrosion challenges. This involves environmentally friendly inhibitors derived from plants, offering a sustainable alternative to conventional chemical treatments. Our inquiry screens and selects inhibitors based on their efficacy in hindering biofilm formation and reducing corrosion rates on the X52 surface. This study contributes valuable insights into the interplay between electrochemical processes and biofilm attachment on the X52 surface. Furthermore, the outcomes of this research have broader implications for the oil and gas industry, where biofilm-related corrosion is a persistent concern. The exploration of eco-friendly inhibitors not only holds promise for corrosion control but also aligns with environmental considerations and sustainability goals. The comprehensive nature of this research aims to enhance our understanding of biofilm dynamics, provide effective strategies for corrosion mitigation, and contribute to sustainable practices in pipeline management within the oil and gas sector.

Keywords: bio-corrosion, biofilm, attachment, X52, metal/bacteria interface

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Authors: D. W. Mohammed, J. Bowen, S. N. Kukureka

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Successful design and fabrication of flexible devices for electrode components requires a low sheet resistance, high optical transmittance, high mechanical reliability. Indium tin oxide (ITO) film is currently the predominant transparent conductive oxide (TCO) film in potential applications such as flexible organic light- emitting diodes, flat-panel displays, solar cells, and thin film transistors (TFTs). However ITO films are too brittle and their resistivity is rather high in some cases compared with ITO/Ag/ ITO, and they cannot completely meet flexible optoelectronic device requirements. Therefore, in this work the mechanical properties of ITO /Ag/ITO multilayer film that deposited on Polyethylene terephthalate (PET) compared with the single layered ITO sample were investigated using bending fatigue, twisting fatigue and thermal cycling experiments. The electrical resistance was monitored during the application of mechanical and thermal loads to see the pattern of relationship between the load and the electrical continuity as a consequent of failure. Scanning electron microscopy and atomic force microscopy were used to provide surface characterization of the mechanically-tested samples. The effective embedment of the Ag layer between upper and lower ITO films led to metallic conductivity and superior flexibility to the single ITO electrode, due to the high failure strain of the ductile Ag layer. These results indicate that flexible ITO/Ag/ITO multilayer electrodes are a promising candidate for use as transparent conductor in flexible displays. They provided significantly reduced sheet resistance compared to ITO, and improved bending and twisting properties both as a function of radius, angle and thermal cycling.

Keywords: ITO/Ag/ITO multilayer, failure strain, mechanical properties, PET

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Authors: Adela Diepoltova, Klara Konecna, Ondrej Jandourek, Petr Nachtigal

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A loss of control over antibiotic-resistant pathogens has become a global issue due to severe and often untreatable infections. This state is reflected in complicated treatment, health costs, and higher mortality. All these factors emphasize the urgent need for the discovery and development of new anti-infectives. One of the most common pathogens mentioned in the phenomenon of antibiotic resistance are bacteria of the genus Staphylococcus. These bacterial agents have developed several mechanisms against the effect of antibiotics. One of them is biofilm formation. In staphylococci, biofilms are associated with infections such as endocarditis, osteomyelitis, catheter-related bloodstream infections, etc. To author's best knowledge, no validated and standardized methodology evaluating candidate compound activity against staphylococcal biofilms exists. However, a variety of protocols for in vitro drug activity testing has been suggested, yet there are often fundamental differences. Based on our experience, a key methodological step that leads to credible results is to form a robust biofilm with appropriate attributes such as firm adherence to the substrate, a complex arrangement in layers, and the presence of extracellular polysaccharide matrix. At first, for the purpose of drug antibiofilm activity evaluation, the focus was put on various conditions (supplementation of cultivation media by human plasma/fetal bovine serum, shaking mode, the density of initial inoculum) that should lead to reproducible and robust in vitro staphylococcal biofilm formation in microtiter plate model. Three model staphylococcal reference strains were included in the study: Staphylococcus aureus (ATCC 29213), methicillin-resistant Staphylococcus aureus (ATCC 43300), and Staphylococcus epidermidis (ATCC 35983). The total biofilm biomass was quantified using the Christensen method with crystal violet, and results obtained from at least three independent experiments were statistically processed. Attention was also paid to the viability of the biofilm-forming staphylococcal cells and the presence of extracellular polysaccharide matrix. The conditions that led to robust biofilm biomass formation with attributes for biofilms mentioned above were then applied by introducing an alternative method analogous to the commercially available test system, the Calgary Biofilm Device. In this test system, biofilms are formed on pegs that are incorporated into the lid of the microtiter plate. This system provides several advantages (in situ detection and quantification of biofilm microbial cells that have retained their viability after drug exposure). Based on our preliminary studies, it was found that the attention to the peg surface and substrate on which the bacterial biofilms are formed should also be paid to. Therefore, further steps leading to the optimization were introduced. The surface of pegs was coated by human plasma, fetal bovine serum, and L-polylysine. Subsequently, the willingness of bacteria to adhere and form biofilm was monitored. In conclusion, suitable conditions were revealed, leading to the formation of reproducible, robust staphylococcal biofilms in vitro for the microtiter model and the system analogous to the Calgary biofilm device, as well. The robustness and typical slime texture could be detected visually. Likewise, an analysis by confocal laser scanning microscopy revealed a complex three-dimensional arrangement of biofilm forming organisms surrounded by an extracellular polysaccharide matrix.

Keywords: anti-biofilm drug activity screening, in vitro biofilm formation, microtiter plate model, the Calgary biofilm device, staphylococcal infections, substrate modification, surface coating

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Authors: Samir El-Gendy, Doaa Zaghloul

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The current study dealt with the gross and microscopic anatomy of the integument of male ostrich in addition to the histological features of different areas of skin by light and SEM. The ostrich skin is characterized by prominent feather follicles and bristles. The number of feather follicles was determined per cm2 in different regions. The integument of ostrich had many modifications which appeared as callosities and scales, nail and toe pads. They were sternal, pubic and Achilles tendon callosities. The vacuolated epidermal cells were seen mainly in the skin of legs and to a lesser extent in the skin of back and Achilles areas. Higher lipogenic potential was expressed by epidermis from glabrous areas of ostrich skin. The dermal papillae were found in the skin of feathered area of neck and back and this was not a common finding in bird's skin which may give resistance against shearing forces in these regions of ostrich skin. The thickness of the keratin layer of ostrich varied, being thick and characteristically loose in the skin at legs, very thin and wavy at neck, while at Achilles skin area, scale and toe pad were thick and more compact, with the thickest very dense and wavy keratin layer at the nail. The dermis consisted of superficial layer of dense irregular connective tissue characterized by presence of many vacuoles of different sizes just under the basal lamina of the epithelium of epidermis and deep layer of dense regular connective tissue. This result suggested presence of fat droplets in this layer which may be to overcome the lack of good barrier of cutaneous water loss in epidermis.

Keywords: ostrich, light microscopy, scanning electron microscopy, integument, skin modifications

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Authors: Erifyli Tsagkari, Stephanie Connelly, Zhaowei Liu, Andrew McBride, William Sloan

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Biofilms play an essential role in treating water in biofiltration systems. The biofilm morphology and function are inextricably linked to the hydrodynamics of flow through a filter, and yet engineers rarely explicitly engineer this interaction. We develop a system that links computer simulation and 3-D printing to optimize and rapidly prototype filter media to optimize biofilm function with the hypothesis that biofilm function is intimately linked to the flow passing through the filter. A computational model that numerically solves the incompressible time-dependent Navier Stokes equations coupled to a model for biofilm growth and function is developed. The model is imbedded in an optimization algorithm that allows the model domain to adapt until criteria on biofilm functioning are met. This is applied to optimize the shape of filter media in a simple flow channel to promote biofilm formation. The computer code links directly to a 3-D printer, and this allows us to prototype the design rapidly. Its validity is tested in flow visualization experiments and by microscopy. As proof of concept, the code was constrained to explore a small range of potential filter media, where the medium acts as an obstacle in the flow that sheds a von Karman vortex street that was found to enhance the deposition of bacteria on surfaces downstream. The flow visualization and microscopy in the 3-D printed realization of the flow channel validated the predictions of the model and hence its potential as a design tool. Overall, it is shown that the combination of our computational model and the 3-D printing can be effectively used as a design tool to prototype filter media to optimize biofilm formation.

Keywords: biofilm, biofilter, computational model, von karman vortices, 3-D printing.

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Authors: Monika Kallubai, Shreya Dubey, Rajagopal Subramanyam

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Our study is all about the biological interactions of synthesized 5β-dihydrocortisol (Dhc) and 5β-dihydrocortisol acetate (DhcA) molecules with carrier protein Human Serum Albumin (HSA). The cytotoxic study was performed on breast cancer cell line (MCF-7) normal human embryonic kidney cell line (HEK293), the IC50 values for MCF-7 cells were 28 and 25 µM, respectively, whereas no toxicity in terms of cell viability was observed with HEK293 cell line. The further experiment proved that Dhc and DhcA induced 35.6% and 37.7% early apoptotic cells and 2.5%, 2.9% late apoptotic cells respectively. Morphological observation of cell death through TUNEL assay revealed that Dhc and DhcA induced apoptosis in MCF-7 cells. The complexes of HSA–Dhc and HSA–DhcA were observed as static quenching, and the binding constants (K) was 4.7±0.03×104 M-1 and 3.9±0.05×104 M-1, and their binding free energies were found to be -6.4 and -6.16 kcal/mol, respectively. The displacement studies confirmed that lidocaine 1.4±0.05×104 M-1 replaced Dhc, and phenylbutazone 1.5±0.05×104 M-1 replaced by DhcA, which explains domain I and domain II are the binding sites for Dhc and DhcA. Further, CD results revealed that the secondary structure of HSA was altered in the presence of Dhc and DhcA. Furthermore, the atomic force microscopy and transmission electron microscopy showed that the dimensions like height and molecular sizes of the HSA–Dhc and HSA–DhcA complex were larger compared to HSA alone. Detailed analysis through molecular dynamics simulations also supported the greater stability of HSA–Dhc and HSA–DhcA complexes, and root-mean-square-fluctuation interpreted the binding site of Dhc as domain IB and domain IIA for DhcA. This information is valuable for the further development of steroid derivatives with improved pharmacological significance as novel anti-cancer drugs.

Keywords: apoptosis, dihydrocortisol, fluorescence quenching, protein conformations

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Authors: Bertilia L. Bartley, Ledjane S. Barreto

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As a preliminary investigation on the control of microcracking in composite cement pastes, this study explores and compares the compatibility of Tetraethyl Orthosilicate (TEOS), Ethylene Glycol (EG) and Silicone Resin (SIL) in cement pastes cured at high temperature. Pastes were prepared by incorporating ordinary Portland cement (OPC) into an additive solution, using a solution/cement ratio of 0.45. Specimens were molded for 24h at 21 ± 2°C, then cured in deionized water for another 24h at 74 ± 1°C. TEOS and EG influence on fresh paste properties were similar to the reference OPC paste yet disintegration was observed in EG and SIL specimens after the first 12h of curing. X-Ray Diffraction analysis (XRD) coupled with thermogravimetric analysis (TGA/DTG) verified that SIL addition impedes portlandite formation significantly. Backscatter Scanning Electron Microscopy (SEM) techniques were therefore performed on selected areas of each sample to investigate the morphology of the hydration products detected. Various morphologies of portlandite crystals were observed in pastes with EG and TEOS addition, as well as dense morphologies of calcium silicate hydrate (C-S-H) gel and fibers, and ettringite needles. However, the formation of portlandite aggregate and clusters of C-S-H was highly favored by TEOS addition. Furthermore, the microstructural details of composite pastes were clearly visible at low magnifications i.e. 500x, as compared to the OPC paste. The results demonstrate accelerated hydration within composite pastes, a uniform distribution of hydration products, as well as an adhesive interaction with the products and polymer additive. Overall, TEOS demonstrated the most favorable influence, which indicates the potential of TEOS as a compatible polymer additive within the cement system at high temperature.

Keywords: accelerated curing, cement/polymer composite, hydration, microstructural properties, morphology, portlandite, scanning electron microscopy (sem)

Procedia PDF Downloads 159

Authors: Fatai O. Oladoyinbo, Felix O. Sanni, Akinwunmi Fatai, Kamoli A. Amusa, Saheed A. Ganiyu, Wasiu B. Ayinde, Tajudeen A. Afolabi, Enock O. Dare

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Silver (Ag) and silica (SiO2) nanoparticles were synthesized using the chemical reduction method from silver nitrate and sodium silicate, respectively. X-ray Diffraction (XRD), High-Resolution Transmission Electron Microscopy (HRTEM), Scanning Electron Microscopy (SEM), Uv-Visible spectroscopy, Energy Dispersive X-ray (EDX) spectroscopy and N2 adsorption-desorption techniques were utilized to characterize the composition and structure of the samples. The crystallinity pattern of Ag nanoparticles was indexed as (111), (200), (220) and (311), which allowed reflections from face-centered cubic silver. XRD of SiO2 showed good porosity with a broad-spectrum band at Bragg’s angle 2θ of 22° while that of Ag-SiO2 showed distinct peaks at 2θ values of 39°, 43°, 66° and 79°. The XRD result agreed perfectly with the SEM and HRTEM images which showed Ag-SiO2 isotropic and anisotropic under the varying concentration of reactants. The elemental composition of Ag-SiO2, as displayed by EDX, confirmed Ag enrichment in the Ag-SiO2 heterostructure. The Uv-Visible peak at 421 nm confirmed the Surface Plasmon Resonance absorption peak of silver nanoparticles. N2 adsorption-desorption result showed a broad band of Ag-SiO2 from 3 to 8 nm, which indicated relatively narrow pore size distributions. Humidity sensing measurements performed in a controlled humidity chamber showed very high sensitivity with a sensitivity factor (SF) of 4.63 and high linearity with a steady decrease in resistance to humidity from 880 Ω at 10% RH to 190 Ω at 100% RH, indicating that Ag-SiO2 nanocomposite is a good sensing material with high sensitivity and linearity.

Keywords: silver, silica, nanocomposite, synthesis, heterostructure, core shell

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Authors: C. Busuioc, S. I. Jinga, E. Pavel

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The continuous need of more non-volatile memories with a higher storage capacity, smaller dimensions and weight, as well as lower costs, has led to the exploration of optical lithography on active media, as well as patterned magnetic composites. In this context, optical lithography is a technique that can provide a significant decrease of the information bit size to the nanometric scale. However, there are some restrictions that arise from the need of breaking the optical diffraction limit. Major achievements have been obtained by employing a vitoceramic material as active medium and a laser beam operated at low power for the direct writing procedure. Thus, optical discs with ultra-high density were fabricated by a conventional melt-quenching method starting from analytical purity reagents. They were subsequently used for 3D recording based on their photosensitive features. Naturally, the next step consists in the elucidation of the composition and structure of the active centers, in correlation with the use of silver and rare-earth compounds for the synthesis of the optical supports. This has been accomplished by modern characterization methods, namely transmission electron microscopy coupled with selected area electron diffraction, scanning transmission electron microscopy and electron energy loss spectroscopy. The influence of laser diode parameters, silver concentration and fluorescent compounds formation on the writing process and final material properties was investigated. The results indicate performances in terms of capacity with two order of magnitude higher than other reported information storage systems. Moreover, the fluorescent photosensitive vitroceramics may be integrated in other applications which appeal to nanofabrication as the driving force in electronics and photonics fields.

Keywords: data storage, fluorescent compounds, laser writing, vitroceramics

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Authors: Arnold S. Freitas Neto, Rodrigo E. Coelho, Erick S. Mendonça

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The study aims to assess if high-purity iron powder in iron-aluminum alloys can be replaced by SAE 1020 steel chips with an atomicity proportion of 50% for each element. Chips of SAE 1020 are rejected in industrial processes. Thus, the use of SAE 1020 as a replaceable composite for iron increase the sustainability of ferrous alloys by recycling industrial waste. The alloys were processed by high energy milling, of which the main advantage is the minimal loss of raw material. The raw material for three of the six samples were high purity iron powder and recyclable aluminum cans. For the other three samples, the high purity iron powder has been replaced with chips of SAE 1020 steel. The process started with the separate milling of chips of aluminum and SAE 1020 steel to obtain the powder. Subsequently, the raw material was mixed in the pre-defined proportions, milled together for five hours and then underwent a closed-die hot compaction at the temperature of 500 °C. Thereafter, the compacted samples underwent heat treatments known as sintering and solubilization. All samples were sintered one hour, and 4 samples were solubilized for either 4 or 10 hours under well-controlled atmosphere conditions. Lastly, the composition and the mechanical properties of their hardness were analyzed. The samples were analyzed by optical microscopy, scanning electron microscopy and hardness testing. The results of the analysis showed a similar chemical composition and interesting hardness levels with low standard deviations. This verified that the use of SAE 1020 steel chips can be a low-cost alternative for high-purity iron powder and could possibly replace high-purity Iron in industrial applications.

Keywords: Fe-Al alloys, high energy milling, iron-aluminum alloys, metallography characterization, powder metallurgy, recycling ferrous alloy, SAE 1020 steel recycling

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Authors: Jung-Hwan Oh, Rajesh Kumar, Il-Kwon Oh

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Porous graphene has extensive potential applications in variety of fields such as hydrogen storage, CO oxidation, gas separation, supercapacitors, fuel cells, nanoelectronics, oil adsorption, and so on. However, the generation of some carbon atoms vacancies for precise small holes have been not extensively studied to prevent the agglomerates of graphene sheets and to obtain porous graphene with high surface area. Recently, many research efforts have been presented to develop physical and chemical synthetic approaches for porous graphene. But physical method has very high cost of manufacture and chemical method consumes so many hours for porous graphene. Herein, we propose a porous graphene contained holes with atomic scale precision by embedding metal nano-particles through microwave irradiation for hydrogen storage and CO oxidation multi- functionalities. This proposed synthetic method is appropriate for fast and convenient production of three dimensional nanostructures, which have nanoholes on the graphene surface in consequence of microwave irradiation. The metal nanoparticles are dispersed quickly on the graphene surface and generated uniform nanoholes on the graphene nanosheets. The morphological and structural characterization of the porous graphene were examined by scanning electron microscopy (SEM), transmission scanning electron microscopy (TEM) and RAMAN spectroscopy, respectively. The metal nanoparticle-embedded porous graphene exhibits a microporous volume of 2.586cm3g-1 with an average pore radius of 0.75 nm. HR-TEM analysis was carried out to further characterize the microstructures. By investigating the RAMAN spectra, we can understand the structural changes of graphene. The results of this work demonstrate a possibility to produce a new class of porous graphene. Furthermore, the newly acquired knowledge for the diffusion into graphene can provide useful guidance for the development of the growth of nanostructure.

Keywords: CO oxidation, hydrogen storage, nanocomposites, porous graphene

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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: Okafor E. Ijeoma, Isimi C. Yetunde, Okoh E. Judith, Kunle O. Olobayo, Emeje O. Martins

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Starch has gained interest as a renewable and environmentally compatible polymer due to the increase in its use. However, starch by itself could not be satisfactorily applied in industrial processes due to some inherent disadvantages such as its hydrophilic character, poor mechanical properties, its inability to withstand processing conditions such as extreme temperatures, diverse pH, high shear rate, freeze-thaw variation and dimensional stability. The range of physical properties of parent starch can be enlarged by chemical modification which invariably enhances their use in a number of applications found in industrial processes and food manufacture. In this study, Manihot esculentus starch was subjected to modification by oxidation. Fourier Transmittance Infra- Red (FTIR) and Raman spectroscopies were used to confirm the synthesis while Scanning Electron Microscopy (SEM) and X- Ray Diffraction (XRD) were used to characterize the new polymer. DPPH (2, 2-diphenyl-1-picryl-hydrazyl-hydrate) free radical assay was used to determine the antioxidant property of the oxidized starch. Our results show that the modification had no significant effect on the foaming capacity as well as on the emulsion capacity. Scanning electron microscopy revealed that oxidation did not alter the predominantly circular-shaped starch granules, while the X-ray pattern of both starch, native and modified were similar. FTIR results revealed a new band at 3007 and 3283cm-1. Differential scanning calorimetry returned two new endothermic peaks in the oxidized starch with an improved gelation capacity and increased enthalpy of gelatinization. The IC50 of oxidized starch was notably higher than that of the reference standard, ascorbic acid.

Keywords: antioxidant activity, DPPH, M. esculentus, oxidation, starch

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Authors: Alexey Yu. Postnikov, Nikolay T. Kazakovskiy, Valery V. Mokrushin, Irina A. Tsareva, Andrey A. Potekhin, Valentina N. Golubeva, Yuliya V. Potekhina, Maxim V. Tsarev

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The development of tritium and deuterium targets for neutron tubes and generators is a part of the activities in All-Russia Research Institute of Experimental Physics (RFNC-VNIIEF). These items contain a metal substrate (for example, copper) with a titanium film with a few microns thickness deposited on it. Then these metal films are saturated with tritium, deuterium or their mixtures. The significant problem in neutron tubes and neutron generators is the characterization of substrate surface before a deposition of titanium film on it, and analysis of the deposited titanium film’s surface before hydrogenation and after a saturation of the film with hydrogen isotopes. The performance effectiveness of neutron tube and generator also depends on upon the quality parameters of the surface of the initial substrate, deposited metal film and hydrogenated target. The objective of our work is to study the target prototype samples, that have differ by various approaches to the preliminary chemical processing of a copper substrate, and to analyze the integrity of titanium film after its saturation with deuterium. The research results of copper substrate and the surface of deposited titanium film with the use of electron microscopy, X-ray spectral microanalysis and laser-spark methods of analyses are presented. The causes of surface defects appearance have been identified. The distribution of deuterium and some impurities (oxygen and nitrogen) along the surface and across the height of the hydrogenated film in the target has been established. This allows us to evaluate the composition homogeneity of the samples and consequently to estimate the quality of hydrogenated samples. As the result of this work the propositions on the advancement of production technology and characterization of target’s surface have been presented.

Keywords: tritium and deuterium targets, titanium film, laser-spark methods, electron microscopy

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Authors: Muhammad Zahid, Ilker S. Bayer, Athanassia Athanassiou

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Fluorinated polymers having C8 chemistry (chemicals with 8 fluorinated carbon atoms) are well renowned for their excellent low surface tension and water repelling properties. However, these polymers degrade into highly toxic heavy perfluoro acids in the environment. When the C8 chemistry is reduced to C6 chemistry, this environmental concern is eliminated at the expense of reduced liquid repellent performance. In order to circumvent this, in this study, we demonstrate pre-treatment of woven cotton fabrics with a fluorinated acrylic copolymer with C6 chemistry and subsequently with a silicone polymer to render them hydrophobic. A commercial fluorinated acrylic copolymer was blended with silica nanoparticles to form hydrophobic nano-roughness on cotton fibers and a second coating layer of polydimethylsiloxane (PDMS) was applied on the fabric. A static water contact angle (for 5µl) and rolling angle (for 12.5µl) of 147°±2° and 31° were observed, respectively. Hydrostatic head measurements were also performed to better understand the performance with 26±1 cm and 2.56kPa column height and static pressure respectively. Fabrication methods (with rod coater etc.) were kept simple, reproducible, and scalable and cost efficient. Moreover, the robustness of applied coatings was also evaluated by sonication cleaning and abrasion methods. Water contact angle (WCA), water shedding angle (WSA), hydrostatic head, droplet bouncing-rolling off and prolonged staining tests were used to characterize hydrophobicity of materials. For chemical and morphological analysis, various characterization methods were used such as attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), atomic force microscopy (AFM) and scanning electron microscopy (SEM).

Keywords: fluorinated polymer, hydrophobic, polydimethylsiloxane, water contact angle

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