Search results for: 4D scanning ultrafast microscopy

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: Ekere E. Kokonne, Isimi C. Yetunde, Okoh E. Judith, Okafor E. Ijeoma, Ajeh J. Isaac, Olobayo O. Kunle, Emeje O. Martins

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NIPRIMAL® is a mono herbal formulation of Nauclea latifolia used in the treatment of malaria. The stability of extracts made from plant material is essential to ensure the quality, safety and efficacy of the finished product. This study assessed the stability of the formulation under three different storage conditions; normal room temperature, infrared and under refrigeration. Differential Scanning Calorimetry (DSC) and Thin Layer Chromatography (TLC) were used to monitor the formulations. The DSC analysis was done from 0oC to 350oC under the three storage conditions. Results obtained indicate that NIPRIMAL® was stable at all the storage conditions investigated. Thin layer chromatography (TLC) after 6 months showed there was no significant difference between retention factor (RF) values for the various storage conditions. The reference sample had four spots with RF values of 0.47, 0.68, 0.76, 0.82 respectively and these spots were retained in the test formulations with corresponding RF values were after 6 months at room temperature and refrigerated temperature been 0.56, 0.73, 0.80, 0.92 and 0.47, 0.68, 0.76, 0.82 respectively. On the other hand, the RF values (0.55, 0.74, 0.77, 0.93) obtained under infrared after 1 month varied slightly from the reference. The sample exposed to infrared had a lower heat capacity compared to that stored under room temperature or refrigeration. A combination of TLC and DSC measurements has been applied for assessing the stability of NIPRIMAL®. Both methods were found to be rapid, sensitive and reliable in determining its stability. It is concluded that NIPRIMAL® can be stored under any of the tested conditions without degradation. This study is a major contribution towards developing appropriate stability monitoring parameters for herbal products.

Keywords: differential scanning calorimetry, formulation, NIPRIMAL®, stability, thin layer hromatography

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Authors: Mohammad Khoshini, Arman Khoshghalb, Meghdad Payan, Nasser Khalili

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Most of the Earth’s crust surface rocks are technically categorized as weak rocks or weakly bonded geomaterials. Deeply weathered, weakly cemented, friable and easily erodible, they demonstrate complex material behaviour and understanding the overlooked mechanical behaviour of such materials is of particular importance in geotechnical engineering practice. Weakly bonded geomaterials are so susceptible to surface shear and moisture that conventional methods of core drilling fail to extract high-quality undisturbed samples out of them. Moreover, most of these geomaterials are of high heterogeneity rendering less reliable and feasible material characterization. In order to compensate for the unpredictability of the material response, either numerous experiments are needed to be conducted or large factors of safety must be implemented in the design process. However, none of these approaches is sustainable. In this study, a method for dry core drilling of such materials is introduced to take high-quality undisturbed core samples. By freezing the material at certain moisture content, a secondary structure is developed throughout the material which helps the whole structure to remain intact during the core drilling process. Moreover, to address the heterogeneity issue, the natural material was reconstructed artificially to obtain a homogeneous material with very high similarity to the natural one in both micro and macro-mechanical perspectives. The method is verified for both micro and macro scale. In terms of micro-scale analysis, using Scanning Electron Microscopy (SEM), pore spaces and inter-particle bonds were investigated and compared between natural and artificial materials. X-Ray Diffraction, XRD, analyses are also performed to control the chemical composition. At the macro scale, several uniaxial compressive strength tests, as well as triaxial tests, were performed to verify the similar mechanical response of the materials. A high level of agreement is observed between micro and macro results of natural and artificially bonded geomaterials. The proposed methods can play an important role to cut down the costs of experimental programs for material characterization and also to promote the accuracy of the numerical modellings based on the experimental results.

Keywords: Artificial geomaterial, core drilling, macro-mechanical behavior, micro-scale, sample preparation, SEM photography, weakly bonded geomaterials

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Authors: Xin Li, Zhenxue Jiang, Zhuo Li

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Generally, shale gas is trapped within shale systems with low porosity and ultralow permeability as free and adsorbing states. Its production is controlled by properties, in terms of occurrence phases, gas contents, and percolation characteristics. These properties are all influenced by porous features. In this paper, porosity differences of marine shales were explored between Lower Cambrian shale and Lower Silurian shale of Sichuan Basin, South China. Both the two shales were marine shales with abundant oil-prone kerogen and rich siliceous minerals. Whereas Lower Cambrian shale (3.56% Ro) possessed a higher thermal degree than that of Lower Silurian shale (2.31% Ro). Samples were measured by a combination of organic-chemistry geology measurement, organic matter (OM) isolation, X-ray diffraction (XRD), N2 adsorption, and focused ion beam milling and scanning electron microscopy (FIB-SEM). Lower Cambrian shale presented relatively low pore properties, with averaging 0.008ml/g pore volume (PV), averaging 7.99m²/g pore surface area (PSA) and averaging 5.94nm average pore diameter (APD). Lower Silurian shale showed as relatively high pore properties, with averaging 0.015ml/g PV, averaging 10.53m²/g PSA and averaging 18.60nm APD. Additionally, fractal analysis indicated that the two shales presented discrepant pore morphologies, mainly caused by differences in the combination of pore types between the two shales. More specifically, OM-hosted pores with pin-hole shape and dissolved pores with dead-end openings were the main types in Lower Cambrian shale, while OM-hosted pore with a cellular structure was the main type in Lower Silurian shale. Moreover, porous characteristics of isolated OM suggested that OM of Lower Silurian shale was more capable than that of Lower Cambrian shale in the aspect of pore contribution. PV of isolated OM in Lower Silurian shale was almost 6.6 times higher than that in Lower Cambrian shale, and PSA of isolated OM in Lower Silurian shale was almost 4.3 times higher than that in Lower Cambrian shale. However, no apparent differences existed among samples with various matrix compositions. At late diagenetic or metamorphic epoch, extensive diagenesis overprints the effects of minerals on pore properties and OM plays the dominant role in pore developments. Hence, differences of porous features between the two marine shales highlight the effect of diagenetic degree on OM-hosted pore development. Consequently, distinctive pore characteristics may be caused by the different degrees of diagenetic evolution, even with similar matrix basics.

Keywords: marine shale, lower Cambrian, lower Silurian, om isolation, pore properties, om-hosted pore

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Authors: Mohamed Ayeldeen, Abdelazim Negm

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Nowadays, strength characteristics of soils have more importance due to increasing building loads. In some projects, geotechnical properties of the soils are be improved using man-made materials varying from cement-based to chemical-based. These materials have proven successful in improving the engineering properties of the soil such as shear strength, compressibility, permeability, bearing capacity etc.. However, the use of these artificial injection formulas often modifies the pH level of soil, contaminates soil and groundwater. This is attributed to their toxic and hazardous characteristics. Recently, an environmentally friendly soil treatment method or Biological Treatment Method (BTM) was to bond particles of loose sandy soils. This research paper presents the preliminary results of using biopolymers for strengthening cohesionless soil. Xanthan gum was identified for further study over a range of concentrations varying from 0.25% to 2.00%. Xanthan gum is a polysaccharide secreted by the bacterium Xanthomonas campestris, used as a food additive and it is a nontoxic material. A series of direct shear, unconfined compressive strength, and permeability tests were carried out to investigate the behavior of sandy soil treated with Xanthan gum with different concentration ratios and at different curing times. Laser microscopy imaging was also conducted to study the microstructure of the treated sand. Experimental results demonstrated the compatibility of Xanthan gum to improve the geotechnical properties of sandy soil. Depending on the biopolymer concentration, it was observed that the biopolymers effectively increased the cohesion intercept and stiffness of the treated sand and reduced the permeability of sand. The microscopy imaging indicates that the cross-links of the biopolymers through and over the soil particles increase with the increase of the biopolymer concentration.

Keywords: biopolymer, direct shear, permeability, sand, shear strength, Xanthan gum

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Authors: Kien Xuan Ngo

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Cassiicolin (Cas), a toxin produced by Corynespora cassiicola, is responsible for corynespora leaf fall (CLF) disease in rubber trees. Currently, the molecular mechanism of the cytotoxicity of Cas isoforms (i.e., Cas1, Cas2) on rubber leaves and its host selectivity have not been fully elucidated. This study analyzed the binding of Cas1 and Cas2 to membranes consisting of different plant lipids and their membrane-disruption activities. Using high-speed atomic force microscopy and confocal microscopy, this study reveals that the binding and disruption activities of Cas1 and Cas2 on lipid membranes are strongly dependent on the specific plant lipids. The negative phospholipids, glycerolipids, and sterols are more susceptible to membrane damage caused by Cas1 and Cas2 than neutral phospholipids and betaine lipids. In summary, This study unveils that (i) Cas1 and Cas2 directly damage and cause necrosis in the leaves of specific rubber clones; (ii) Cas1 and Cas2 can form biofilm-like structures on specific lipid membranes (negative phospholipids, glycerolipids, and sterols). The biofilm-like formation of Cas toxin plays an important role in selective disruption on lipid membranes; (iii) Vulnerability of the specific cytoplasmic membranes to the selective Cas toxin is the most remarkable feature of cytotoxicity of Cas toxin on plant cells. Finally, researcher’s exploration is crucial to understand the basic molecular mechanism underlying the host-selective toxic interaction of Cas toxin with cytoplasmic membranes in plant cells.

Keywords: cassiicolin, corynespora leaf fall disease, high-speed AFM, giant liposome vesicles

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Authors: Muhammad Habib, Lin Tang, Guoliang Xue, Attaur Rahman, Myong-Ho Kim, Soonil Lee, Xuefan Zhou, Yan Zhang, Dou Zhang

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Designing a high-performance, lead-free ceramic has become a cutting-edge research topic due to growing concerns about the toxic nature of lead-based materials. In this work, a convenient strategy of compositional design and domain engineering is applied to the lead-fee BiFeO₃-BaTiO₃ ceramics, which provides a flexible polarization-free-energy profile for domain switching. Here, simultaneously enhanced dynamic piezoelectric constant (d33* = 772 pm/V) and a good thermal-stability (d33* = 26% over the temperature of 20-180 ᵒC) are achieved with a high Curie temperature (TC) of 432 ᵒC. This high piezoelectric strain performance is collectively attributed to multiple effects such as thermal quenching, suppression of defect charges by donor doping, chemically induced local structure heterogeneity, and electric field-induced phase transition. Furthermore, the addition of BT content decreased octahedral tilting, reduced anisotropy for domain switching and increased tetragonality (cₜ/aₜ), providing a wider polar length for B-site cation displacement, leading to high piezoelectric strain performance. Atomic-resolution transmission electron microscopy and piezoelectric force microscopy combined with X-ray diffraction results strongly support the origin of high piezoelectricity. The high and temperature-stable piezoelectric strain response of this work is superior to those of other lead-free ceramics. The synergistic approach of composition design and the concept present here for the origin of high strain response provides a paradigm for the development of materials for high-temperature piezoelectric actuator applications.

Keywords: Piezoelectric, BiFeO3-BaTiO3, Quenching, Temperature-insensitive

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Authors: Raghuram Kandimalla, Sanjeeb Kalita, Bhaswati Choudhury, Jibon Kotoky

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The quest for developing an ideal suture material prompted our interest to develop a novel suture with advantageous characteristics to market available ones. We developed novel suture biomaterial from muga silk (Antheraea assama) and ramie (Boehmeria nivea) plant fiber. Field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), attenuated total reflection fourier transform infrared spectroscopy (ATR-FTIR) and thermo gravimetric analysis (TGA) results revealed the physicochemical properties of the fibers which supports the suitability of fibers for suture fabrication. Tensile properties of the prepared sutures were comparable with market available sutures and it found to be biocompatible towards human erythrocytes and nontoxic to mammalian cells. The prepared sutures completely healed the superficial deep wound incisions within seven days in adult male wister rats leaving no rash and scar. Histopathology studies supports the wound healing ability of sutures, as rapid synthesis of collagen, connective tissue and other skin adnexal structures were observed within seven days of surgery. Further muga suture surface modified by exposing the suture to oxygen plasma which resulted in formation of nanotopography on suture surface. Broad spectrum antibiotic amoxicillin was functionalized on the suture surface to prepare an advanced antimicrobial muga suture. Surface hydrophilicity induced by oxygen plasma results in an increase in drug-impregnation efficiency of modified muga suture by 16.7%. In vitro drug release profiles showed continuous and prolonged release of amoxicillin from suture up to 336 hours. The advanced muga suture proves to be effective against growth inhibition of Staphylococcus aureus and Escherichia coli, whereas normal muga suture offers no antibacterial activity against both types of bacteria. In vivo histopathology studies and colony-forming unit count data revealed accelerated wound healing activity of advanced suture over normal one through rapid synthesis and proliferation of collagen, hair follicle and connective tissues.

Keywords: sutures, biomaterials, silk, Ramie

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Authors: Vaibhav Budhiraja, Chandra Mouli Pandey

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The ultrasonic synthesis of nanostructured conducting copolymer is an effective technique to synthesize polymer with desired chemical properties. This tailored nanostructure, shows tremendous improvement in sensitivity and stability to detect a variety of analytes. The present work reports ultrasonically synthesized nanostructured conducting poly(o-phenylenediamine)-co-poly(1-naphthylamine) (POPD-co-PNA). The synthesized material has been characterized using Fourier transform infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy, transmission electron microscopy, X-ray diffraction and cyclic voltammetry. FTIR spectroscopy confirmed random copolymerization, while UV-visible studies reveal the variation in polaronic states upon copolymerization. High crystallinity was achieved via ultrasonic synthesis which was confirmed by X-ray diffraction, and the controlled morphology of the nanostructures was confirmed by transmission electron microscopy analysis. Cyclic voltammetry shows that POPD-co-PNA has rather high electrochemical activity. This behavior was explained on the basis of variable orientations adopted by the conducting polymer chains. The synthesized material was electrophoretically deposited at onto indium tin oxide coated glass substrate which is used as cathode and parallel platinum plate as the counter electrode. The fabricated bioelectrode was further used for detection of glucose by crosslinking of glucose oxidase in the PODP-co-PNA film. The bioelectrode shows a surface-controlled electrode reaction with the electron transfer coefficient (α) of 0.72, charge transfer rate constant (ks) of 21.77 s⁻¹ and diffusion coefficient 7.354 × 10⁻¹⁵ cm²s⁻¹.

Keywords: conducting, electrophoretic, glucose, poly (o-phenylenediamine), poly (1-naphthylamine), ultrasonic

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Authors: Magdalena Diaka, Paweł Mazierski, Joanna Żebrowska, Michał Winiarski, Tomasz Klimczuk, Adriana Zaleska-Medynska

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During the last years, TiO2 nanotubes have been widely studied due to their unique highly ordered array structure, unidirectional charge transfer and higher specific surface area compared to conventional TiO2 powder. These photoactive materials, in the form of thin layer, can be activated by low powered and low cost irradiation sources (such as LEDs) to remove VOCs, microorganism and to deodorize air streams. This is possible due to their directly growth on a support material and high surface area, which guarantee enhanced photon absorption together with an extensive adsorption of reactant molecules on the photocatalyst surface. TiO2 nanotubes exhibit also lots of other attractive properties, such as potential enhancement of electron percolation pathways, light conversion, and ion diffusion at the semiconductor-electrolyte interface. Pure TiO2 nanotubes were previously used to remove organic compounds from the gas phase as well as in water splitting reaction. The major factors limiting the use of TiO2 nanotubes, which have not been fully overcome, are their relatively large band gap (3-3,2 eV) and high recombination rate of photogenerated electron–hole pairs. Many different strategies were proposed to solve this problem, however titania nanostructures containing incorporated metal oxides like Ag2O shows very promising, new optical and photocatalytic properties. Unfortunately, there is still very limited number of reports regarding application of TiO2/MxOy nanostructures. In the present work, we prepared TiO2/Ag2O nanotubes obtained by anodization of Ti-Ag alloys containing 5, 10 and 15 wt. % Ag. Photocatalysts prepared in this way were characterized by X-ray diffraction spectroscopy (XRD), scanning electron microscopy (SEM), luminescence spectroscopy and UV-Vis spectroscopy. The activities of new TiO2/Ag2O were examined by photocatalytic degradation of toluene in gas phase reaction and phenol in aqueous phase using 1000 W Xenon lamp (Oriel) and light emitting diodes (LED) as a irradiation sources. Additionally efficiency of bacteria (Pseudomonas aeruginosa) removal from the gas phase was estimated. The number of surviving bacteria was determined by the serial twofold dilution microtiter plate method, in Tryptic Soy Broth medium (TSB, GibcoBRL).

Keywords: photocatalysis, antibacterial properties, titania nanotubes, new TiO2/MxOy nanostructures

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Authors: Ibrahim Sengor, Sumeyye Cesur, Ilyas Kartal, Faik Nuzhet Oktar, Nazmi Ekren, Ahmet Talat Inan, Oguzhan Gunduz

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In recent years, many researchers focused on nano-size fiber production. Nanofibers have been studied due to their different and superior physical, chemical and mechanical properties. Poly (lactic acid) (PLA), is a type of biodegradable thermoplastic polyester derived from renewable sources used in biomedical owing to its biocompatibility and biodegradability. In addition, zinc oxide is an antibacterial material and hazelnut shell powder is a filling material. In this study, nanofibers were obtained by adding of different ratio Zinc oxide, (ZnO) and hazelnut shell powder at different concentration into Poly (lactic acid) (PLA) by using electrospinning method which is the most common method to obtain nanofibers. After dissolving the granulated polylactic acids in % 1,% 2,% 3 and% 4 with chloroform solvent, they are homogenized by adding tween and hazelnut shell powder at different ratios and then by electrospinning, nanofibers are obtained. Scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FTIR), Differential scanning calorimeter (DSC) and physical analysis such as density, electrical conductivity, surface tension, viscosity measurement and antimicrobial test were carried out after production process. The resulting structures of the nanofiber possess antimicrobial and antiseptic properties, which are attractive for biomedical applications. The resulting structures of the nanofiber possess antimicrobial, non toxic, self-cleaning and rigid properties, which are attractive for biomedical applications.

Keywords: electrospinning, hazelnut shell powder, nanofibers, poly (lactic acid), zinc oxide

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Authors: Madhawa Basnayaka, Jouni Paltakari

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Fully passive backscattering chipless RFID tags are an emerging wireless technology with low cost, higher reading distance, and fast automatic identification without human interference, unlike already available technologies like optical barcodes. The design optimization of chipless RFID tags is crucial as it requires replacing integrated chips found in conventional RFID tags with printed geometric designs. These designs enable data encoding and decoding through backscattered electromagnetic (EM) signatures. The applications of chipless RFID tags have been limited due to the constraints of data encoding capacity and the ability to design accurate yet efficient configurations. The traditional approach to accomplishing design parameters for a desired EM response involves iterative adjustment of design parameters and simulating until the desired EM spectrum is achieved. However, traditional numerical simulation methods encounter limitations in optimizing design parameters efficiently due to the speed and resource consumption. In this work, a deep learning neural network (DNN) is utilized to establish a correlation between the EM spectrum and the dimensional parameters of nested centric rings, specifically square and octagonal. The proposed bi-directional DNN has two simultaneously running neural networks, namely spectrum prediction and design parameters prediction. First, spectrum prediction DNN was trained to minimize mean square error (MSE). After the training process was completed, the spectrum prediction DNN was able to accurately predict the EM spectrum according to the input design parameters within a few seconds. Then, the trained spectrum prediction DNN was connected to the design parameters prediction DNN and trained two networks simultaneously. For the first time in chipless tag design, design parameters were predicted accurately after training bi-directional DNN for a desired EM spectrum. The model was evaluated using a randomly generated spectrum and the tag was manufactured using the predicted geometrical parameters. The manufactured tags were successfully tested in the laboratory. The amount of iterative computer simulations has been significantly decreased by this approach. Therefore, highly efficient but ultrafast bi-directional DNN models allow rapid and complicated chipless RFID tag designs.

Keywords: artificial intelligence, chipless RFID, deep learning, machine learning

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Authors: Elenice Maria Schons Silva, Andre Carlos Silva

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The crescent demand for raw material has increased mining activities. Mineral industry faces the challenge of process more complexes ores, with very small particles and low grade, together with constant pressure to reduce production costs and environment impacts. Froth flotation deserves special attention among the concentration methods for mineral processing. Besides its great selectivity for different minerals, flotation is a high efficient method to process fine particles. The process is based on the minerals surficial physicochemical properties and the separation is only possible with the aid of chemicals such as collectors, frothers, modifiers, and depressants. In order to use sustainable and eco-friendly reagents, oils extracted from three different vegetable species (pequi’s pulp, macauba’s nut and pulp, and Jatropha curcas) were studied and tested as apatite collectors. Since the oils are not soluble in water, an alkaline hydrolysis (or saponification), was necessary before their contact with the minerals. The saponification was performed at room temperature. The tests with the new collectors were carried out at pH 9 and Flotigam 5806, a synthetic mix of fatty acids industrially adopted as apatite collector manufactured by Clariant, was used as benchmark. In order to find a feasible replacement for cornstarch the flour and starch of a graniferous variety of sorghum was tested as depressant. Apatite samples were used in the flotation tests. XRF (X-ray fluorescence), XRD (X-ray diffraction), and SEM/EDS (Scanning Electron Microscopy with Energy Dispersive Spectroscopy) were used to characterize the apatite samples. Zeta potential measurements were performed in the pH range from 3.5 to 12.5. A commercial cornstarch was used as depressant benchmark. Four depressants dosages and pH values were tested. A statistical test was used to verify the pH, dosage, and starch type influence on the minerals recoveries. For dosages equal or higher than 7.5 mg/L, pequi oil recovered almost all apatite particles. In one hand, macauba’s pulp oil showed excellent results for all dosages, with more than 90% of apatite recovery, but in the other hand, with the nut oil, the higher recovery found was around 84%. Jatropha curcas oil was the second best oil tested and more than 90% of the apatite particles were recovered for the dosage of 7.5 mg/L. Regarding the depressant, the lower apatite recovery with sorghum starch were found for a dosage of 1,200 g/t and pH 11, resulting in a recovery of 1.99%. The apatite recovery for the same conditions as 1.40% for sorghum flour (approximately 30% lower). When comparing with cornstarch at the same conditions sorghum flour produced an apatite recovery 91% lower.

Keywords: collectors, depressants, flotation, mineral processing

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Authors: S. Mamoucha, J. Rahul, N. Christodoulakis

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Introduction: Nature has been the source of medicinal agents since the dawn of the human existence on Earth. Currently, millions of people, in the developing world, rely on medicinal plants for primary health care, income generation and lifespan improvement. In Greece, more than 5500 plant taxa are reported while about 250 of them are considered to be of great pharmaceutical importance. Among the plants used for medical purposes, Vitex agnus-castus L. (Verbenaceae) is known since ancient times. It is a small tree or shrub, widely distributed in the Mediterranean basin up to the Central Asia. It is also known as chaste tree or monks pepper. Theophrastus mentioned the shrub several times, as ‘agnos’ in his ‘Enquiry into Plants’. Dioscorides mentioned the use of V. agnus-castus for the stimulation of lactation in nursing mothers and the treatment of several female disorders. The plant has important medicinal properties and a long tradition in folk medicine as an antimicrobial, diuretic, digestive and insecticidal agent. Materials and methods: Leaves were cleaned, detached, fixed, sectioned and investigated with light and Scanning Electron Microscopy (SEM). Histochemical tests were executed as well. Specific histochemical reagents (osmium tetroxide, H2SO4, vanillin/HCl, antimony trichloride, Wagner’ s reagent, Dittmar’ s reagent, potassium bichromate, nitroso reaction, ferric chloride and di methoxy benzaldehyde) were used for the sub cellular localization of secondary metabolites. Results: Light microscopical investigations of the elongated leaves of V. agnus-castus revealed three layers of palisade parenchyma, just below the single layered adaxial epidermis. The spongy parenchyma is rather loose. Adaxial epidermal cells are larger in magnitude, compared to those of the abaxial epidermis. Four different types of capitate, secreting trichomes, were localized among the abaxial epidermal cells. Stomata were observed at the abaxial epidermis as well. SEM revealed the interesting arrangement of trichomes. Histochemical treatment on fresh and plastic embedded tissue sections revealed the nature and the sites of secondary metabolites accumulation (flavonoids, steroids, terpenes). Acknowledgment: This work was supported by IKY - State Scholarship Foundation, Athens, Greece.

Keywords: Vitex agnus-castus, leaf anatomy, histochemical reagents, secondary metabolites

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Authors: Z. Terzopoulou, I. Koliakou, D. Bikiaris

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Tissue engineering offers a new approach to regenerate diseased or damaged tissues such as bone. Great effort is devoted to eliminating the need of removing non-degradable implants at the end of their life span, with biodegradable polymers playing a major part. Poly(ε-caprolactone) (PCL) is one of the best candidates for this purpose due to its high permeability, good biodegradability and exceptional biocompatibility, which has stimulated extensive research into its potential application in the biomedical fields. However, PCL degrades much slower than other known biodegradable polymers and has a total degradation of 2-4 years depending on the initial molecular weight of the device. This is due to its relatively hydrophobic character and high crystallinity. Consequently, much attention has been given to the tunable degradation of PCL to meet the diverse requirements of biomedicine. Poly(ε-caprolactone) (PCL) is a biodegradable polyester that lacks bioactivity, so when used in bone tissue engineering, new bone tissue cannot bond tightly on the polymeric surface. Therefore, it is important to incorporate reinforcing fillers into PCL matrix in order to result in a promising combination of bioactivity, biodegradability, and strength. Natural clay halloysite nanotubes (HNTs) were incorporated into PCL polymeric matrix, via in situ ring-opening polymerization of caprolactone, in concentrations 0.5, 1 and 2.5 wt%. Both unmodified and modified with aminopropyltrimethoxysilane (APTES) HNTs were used in this study. The effect of nanofiller concentration and functionalization with end-amino groups on the physicochemical properties of the prepared nanocomposites was studied. Mechanical properties were found enhanced after the incorporation of nanofillers, while the modification increased further the values of tensile and impact strength. Thermal stability of PCL was not affected by the presence of nanofillers, while the crystallization rate that was studied by Differential Scanning Calorimetry (DSC) and Polarized Light Optical Microscopy (POM) increased. All materials were subjected to enzymatic hydrolysis in phosphate buffer in the presence of lipases. Due to the hydrophilic nature of HNTs, the biodegradation rate of nanocomposites was higher compared to neat PCL. In order to confirm the effect of hydrophilicity, contact angle measurements were also performed. In vitro biomineralization test confirmed that all samples were bioactive as mineral deposits were detected by X-ray diffractometry after incubation in SBF. All scaffolds were tested in relevant cell culture using osteoblast-like cells (MG-63) to demonstrate their biocompatibility

Keywords: biomaterials, nanocomposites, scaffolds, tissue engineering

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Authors: Paresh Patel, Priya Patel, Vaidehi Sorathiya, Navin Sheth

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The aim of present work was to fabricate Salmeterol Xinafoate (SX) metered dose inhaler (MDI) for asthma and to evaluate the SX loaded solid lipid nanoparticles (SLNs) for pulmonary delivery. Solid lipid nanoparticles can be used to deliver particles to the lungs via MDI. A modified solvent emulsification diffusion technique was used to prepare Salmeterol Xinafoate loaded solid lipid nanoparticles by using compritol 888 ATO as lipid, tween 80 as surfactant, D-mannitol as cryoprotecting agent and L-leucine was used to improve aerosolization behaviour. Box-Behnken design was applied with 17 runs. 3-D surface response plots and contour plots were drawn and optimized formulation was selected based on minimum particle size and maximum % EE. % yield, in vitro diffusion study, scanning electron microscopy, X-ray diffraction, DSC, FTIR also characterized. Particle size, zeta potential analyzed by Zetatrac particle size analyzer and aerodynamic properties was carried out by cascade impactor. Pre convulsion time was examined for control group, treatment group and compare with marketed group. MDI was evaluated for leakage test, flammability test, spray test and content per puff. By experimental design, particle size and % EE found to be in range between 119-337 nm and 62.04-76.77% by solvent emulsification diffusion technique. Morphologically, particles have spherical shape and uniform distribution. DSC & FTIR study showed that no interaction between drug and excipients. Zeta potential shows good stability of SLNs. % respirable fraction found to be 52.78% indicating reach to the deep part of lung such as alveoli. Animal study showed that fabricated MDI protect the lungs against histamine induced bronchospasm in guinea pigs. MDI showed sphericity of particle in spray pattern, 96.34% content per puff and non-flammable. SLNs prepared by Solvent emulsification diffusion technique provide desirable size for deposition into the alveoli. This delivery platform opens up a wide range of treatment application of pulmonary disease like asthma via solid lipid nanoparticles.

Keywords: salmeterol xinafoate, solid lipid nanoparticles, box-behnken design, solvent emulsification diffusion technique, pulmonary delivery

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Authors: Manjinder Singh, Jasvinder Singh

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Existing theories of Titanic/Liberty ship, Sydney bridge accidents and practical experience generated an interest in developing weldments those has high toughness under sub-zero temperature conditions. The purpose was to protect the joint from undergoing DBT (Ductile to brittle transition), when ambient temperature reach sub-zero levels. Metallurgical improvement such as low carbonization or addition of deoxidization elements like Mn and Si was effective to prevent fracture in weldments (crack) at low temperature. In the present research, an attempt has been made to investigate the reason behind ductile to brittle transition of mild steel weldments when subjected to sub-zero temperatures and method of its mitigation. Nickel is added to weldments using manual metal arc welding (MMAW) preventing the DBT, but progressive reduction in charpy impact values as temperature is lowered. The variation in toughness with respect to nickel content being added to the weld pool is analyzed quantitatively to evaluate the rise in toughness value with increasing nickel amount. The impact performance of welded specimens was evaluated by Charpy V-notch impact tests at various temperatures (20 °C, 0 °C, -20 °C, -40 °C, -60 °C). Notch is made in the weldments, as notch sensitive failure is particularly likely to occur at zones of high stress concentration caused by a notch. Then the effect of nickel to weldments is investigated at various temperatures was studied by mechanical and metallurgical tests. It was noted that a large gain in impact toughness could be achieved by adding nickel content. The highest yield strength (462J) in combination with good impact toughness (over 220J at – 60 °C) was achieved with an alloying content of 16 wt. %nickel. Based on metallurgical behavior it was concluded that the weld metals solidify as austenite with increase in nickel. The microstructure was characterized using optical and high resolution SEM (scanning electron microscopy). At inter-dendritic regions mainly martensite was found. In dendrite core regions of the low carbon weld metals a mixture of upper bainite, lower bainite and a novel constituent coalesced bainite formed. Coalesced bainite was characterized by large bainitic ferrite grains with cementite precipitates and is believed to form when the bainite and martensite start temperatures are close to each other. Mechanical properties could be rationalized in terms of micro structural constituents as a function of nickel content.

Keywords: MMAW, Toughness, DBT, Notch, SEM, Coalesced bainite

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Authors: Huixia Shi, Can Hu, Jun Zhu, Hongling Guo, Haiyan Li, Hongyan Du

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The identification of human body fluids during forensic investigations is a critical step to determine key details, and present strong evidence to testify criminal in a case. With the popularity of DNA and improved detection technology, the potential question must be revolved that whether the suspect’s DNA derived from saliva or semen, menstrual or peripheral blood, how to identify the red substance or aged blood traces on the spot is blood; How to determine who contribute the right one in mixed stains. In recent years, molecular approaches have been developing increasingly on mRNA, miRNA, DNA methylation and microbial markers, but appear expensive, time-consuming, and destructive disadvantages. Physicochemical methods are utilized frequently such us scanning electron microscopy/energy spectroscopy and X-ray fluorescence and so on, but results only showing one or two characteristics of body fluid itself and that out of working in unknown or mixed body fluid stains. This paper focuses on using chemistry methods Raman spectroscopy and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry to discriminate species of peripheral blood, menstrual blood, semen, saliva, vaginal secretions, urine or sweat. Firstly, non-destructive, confirmatory, convenient and fast Raman spectroscopy method combined with more accurate matrix-assisted laser desorption/ionization time-of-flight mass spectrometry method can totally distinguish one from other body fluids. Secondly, 11 spectral signatures and specific metabolic molecules have been obtained by analysis results after 70 samples detected. Thirdly, Raman results showed peripheral and menstrual blood, saliva and vaginal have highly similar spectroscopic features. Advanced statistical analysis of the multiple Raman spectra must be requested to classify one to another. On the other hand, it seems that the lactic acid can differentiate peripheral and menstrual blood detected by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry, but that is not a specific metabolic molecule, more sensitivity ones will be analyzed in a forward study. These results demonstrate the great potential of the developed chemistry methods for forensic applications, although more work is needed for method validation.

Keywords: body fluids, identification, Raman spectroscopy, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

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Authors: Olumuyiwa Ayoola Kokapi, Olugbenga Solomon Bello

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Dyes are organic compounds with complex aromatic molecular structure that resulted in fast colour on a substance. Dye effluent found in wastewater generated from the dyeing industries is one of the greatest contributors to water pollution. Groundnut hull (GH) is an agricultural material that constitutes waste in the environment. Environmental contamination by hazardous organic chemicals is an urgent problem, which is partially solved through adsorption technologies. The choice of groundnut hull was promised on the understanding that some materials of agricultural origin have shown potentials to act as Adsorbate for hazardous organic chemicals. The aim of this research is to evaluate the potential of groundnut hull to adsorb Crystal violet dye through kinetic, isotherm and thermodynamic studies. The prepared groundnut hulls was characterized using Brunauer, Emmett and Teller (BET), Fourier transform infrared (FTIR) and scanning electron microscopy (SEM). Operational parameters such as contact time, initial dye concentration, pH, and effect of temperature were studied. Equilibrium time for the adsorption process was attained in 80 minutes. Adsorption isotherms used to test the adsorption data were Langmuir and Freundlich isotherms model. Thermodynamic parameters such as ∆G°, ∆H°, and ∆S° of the adsorption processes were determined. The results showed that the uptake of dye by groundnut hulls occurred at a faster rate, corresponding to an increase in adsorption capacity at equilibrium time of 80 min from 0.78 to 4.45 mg/g and 0.77 to 4.45mg/g with an increase in the initial dye concentration from 10 to 50 mg/L for pH 3.0 and 8.0 respectively. High regression values obtained for pseudo-second-order kinetic model, sum of square error (SSE%) values along with strong agreement between experimental and calculated values of qe proved that pseudo second-order kinetic model fitted more than pseudo first-order kinetic model. The result of Langmuir and Freundlich model showed that the adsorption data fit the Langmuir model more than the Freundlich model. Thermodynamic study demonstrated the feasibility, spontaneous and endothermic nature of the adsorption process due to negative values of free energy change (∆G) at all temperatures and positive value of enthalpy change (∆H) respectively. The positive values of ∆S showed that there was increased disorderliness and randomness at the solid/solution interface of crystal violet dye and groundnut hulls. The present investigation showed that, groundnut hulls (GH) is a good low-cost alternative adsorbent for the removal of Crystal Violet (CV) dye from aqueous solution.

Keywords: adsorption, crystal violet dye, groundnut halls, kinetics

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Authors: Inês N. Peça , A. Bicho, Rui Gardner, M. Margarida Cardoso

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Inorganic/organic nanocomplexes offer tremendous scope for future biomedical applications, including imaging, disease diagnosis and drug delivery. The combination of Fe3O4 with biocompatible polymers to produce smart drug delivery systems for use in pharmaceutical formulation present a powerful tool to target anti-cancer drugs to specific tumor sites through the application of an external magnetic field. In the present study, we focused on the evaluation of the effect of the magnetic field application time on the rate of drug release from iron oxide polymeric nanoparticles. Doxorubicin, an anticancer drug, was selected as the model drug loaded into the nanoparticles. Nanoparticles composed of poly(d-lactide-co-glycolide (PLGA), a biocompatible polymer already approved by FDA, containing iron oxide nanoparticles (MNP) for magnetic targeting and doxorubicin (DOX) were synthesized by the o/w solvent extraction/evaporation method and characterized by scanning electron microscopy (SEM), by dynamic light scattering (DLS), by inductively coupled plasma-atomic emission spectrometry and by Fourier transformed infrared spectroscopy. The produced particles yielded smooth surfaces and spherical shapes exhibiting a size between 400 and 600 nm. The effect of the magnetic doxorubicin loaded PLGA nanoparticles produced on cell viability was investigated in mammalian CHO cell cultures. The results showed that unloaded magnetic PLGA nanoparticles were nontoxic while the magnetic particles without polymeric coating show a high level of toxicity. Concerning the therapeutic activity doxorubicin loaded magnetic particles cause a remarkable enhancement of the cell inhibition rates compared to their non-magnetic counterpart. In vitro drug release studies performed under a non-permanent magnetic field show that the application time and the on/off cycle duration have a great influence with respect to the final amount and to the rate of drug release. In order to determine the mechanism of drug release, the data obtained from the release curves were fitted to the semi-empirical equation of the the Korsmeyer-Peppas model that may be used to describe the Fickian and non-Fickian release behaviour. Doxorubicin release mechanism has shown to be governed mainly by Fickian diffusion. The results obtained show that the rate of drug release from the produced magnetic nanoparticles can be modulated through the magnetic field time application.

Keywords: drug delivery, magnetic nanoparticles, PLGA nanoparticles, controlled release rate

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Authors: M. Fatmi, T. Chihi, M. A. Ghebouli, B. Ghebouli

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This work presents the experimental results of the differential scanning calorimetry (DSC), hardness measurements (Hv) and XRD analysis, for order to investigate the kinetics of precipitation phenomena in Al-7%wt. Mg alloy. In the XRD and DSC curves indicates the formation of the intermediate precipitation of β-(Al3Mg2) phase respectively. The activation energies associated with the processes have been determined according to the three models proposed by Kissinger, Ozawa, and Boswell. Consequently, the nucleation mechanism of the precipitates can be explained. These phases are confirmed by XRD analysis.

Keywords: discontinuous precipitation, hardening, Al–Mg alloys, mechanical and mechatronics engineering

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Authors: Agata Zakrzewska, Dominik Kopeć, Adrian Ochtyra

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The growing number of new cameras, sensors, and research methods allow for a broader application of thermal data in remote sensing vegetation studies. The aim of this research was to check whether it is possible to use thermal infrared data with a spectral range (3.6-4.9 μm) obtained during the day and the night to assess the health condition of selected species of deciduous trees in an urban environment. For this purpose, research was carried out in the city center of Warsaw (Poland) in 2020. During the airborne data acquisition, thermal data, laser scanning, and orthophoto map images were collected. Synchronously with airborne data, ground reference data were obtained for 617 studied species (Acer platanoides, Acer pseudoplatanus, Aesculus hippocastanum, Tilia cordata, and Tilia × euchlora) in different health condition states. The results were as follows: (i) healthy trees are cooler than trees in poor condition and dying both in the daytime and nighttime data; (ii) the difference in the canopy temperatures between healthy and dying trees was 1.06oC of mean value on the nighttime data and 3.28oC of mean value on the daytime data; (iii) condition classes significantly differentiate on both daytime and nighttime thermal data, but only on daytime data all condition classes differed statistically significantly from each other. In conclusion, the aerial thermal data can be considered as an alternative to hyperspectral data, a method of assessing the health condition of trees in an urban environment. Especially data obtained during the day, which can differentiate condition classes better than data obtained at night. The method based on thermal infrared and laser scanning data fusion could be a quick and efficient solution for identifying trees in poor health that should be visually checked in the field.

Keywords: middle wave infrared, thermal imagery, tree discoloration, urban trees

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Authors: Lucas Kurth de Azambuja, Loise Silveira da Silva, Gean Vitor Salmoria, Darlan Dallacosta, Carlos Rodrigo de Mello Roesler

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This work provides a physicochemical and thermal characterization assessment of three different hyaluronic acid (HA)-based injections used for rejuvenation skin treatments. The three products analyzed are manufactured by the same manufacturer and commercialized for application on different skin levels. According to the manufacturer, all three HA-based injections are crosslinked and have a concentration of 23 mg/mL of HA, and 0.3% of lidocaine. Samples were characterized by Fourier-transformed infrared (FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and scanning electron microscope (SEM) techniques. FTIR analysis resulted in a similar spectrum when comparing the different products. DSC analysis demonstrated that the fusion points differ in each product, with a higher fusion temperature observed in specimen A, which is used for subcutaneous applications, when compared with B and C, which are used for the middle dermis and deep dermis, respectively. TGA data demonstrated a considerable mass loss at 100°C, which means that the product has more than 50% of water in its composition. TGA analysis also showed that Specimen A had a lower mass loss at 100°C when compared to Specimen C. A mass loss of around 220°C was observed on all samples, characterizing the presence of hyaluronic acid. SEM images displayed a similar structure on all samples analyzed, with a thicker layer for Specimen A when compared with B and C. This series of analyses demonstrated that, as expected, the physicochemical and thermal properties of the products differ according to their application. Furthermore, to better characterize the crosslinking degree of each product and their mechanical properties, a set of different techniques should be applied in parallel to correlate the results and, thereby, relate injection application with material properties.

Keywords: hyaluronic acid, characterization, soft-tissue fillers, injectable gels

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Authors: Kamrun N. Keya, Nasrin A. Kona, Ruhul A. Khan

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Pineapple leaf fiber (PALF) reinforced polypropylene (PP) based composites were fabricated by a conventional compression molding technique. In this investigation, PALF composites were manufactured using different percentages of fiber, which were varying from 25-50% on the total weight of the composites. To fabricate the PALF/PP composites, untreated and treated fibers were selected. A systematic study was done to observe the physical, mechanical and interfacial behavior of the composites. In this study, mechanical properties of the composites such as tensile, impact and bending properties were observed precisely. It was found that 45wt% of fiber composites showed better mechanical properties than others. Maximum tensile strength (TS) and bending strength (BS) was observed, 65 MPa and 50 MPa respectively, whereas the highest tensile modulus (TM) and bending modulus (BM) was examined, 1.7 GPa and 0.85 GPa respectively. The PALF/PP based composites were treated with irradiated under gamma radiation (the source strength 50 kCi Cobalt-60) of various doses (2.5 kGy to 10 kGy). The effect of gamma radiation on the composites was also investigated, and it found that the effect of 5.0 kGy (i.e. units for radiation measurement is 'gray', kGy=kilogray ) gamma dose showed better mechanical properties than other doses. The values of TS, BS, TM, and BM of the irradiated (5.0 kGy) composites were found to improve by 19%, 23%, 17% and 25 % over non-irradiated composites. After flexural testing, fracture sides of the untreated and treated both composites were studied by scanning electron microscope (SEM). SEM results of the treated PALF/PP based composites showed better fiber-matrix adhesion and interfacial bonding than untreated PALF/PP based composites. Water uptake and soil degradation tests of untreated and treated composites were also investigated.

Keywords: PALF, polypropylene, compression molding technique, gamma radiation, mechanical properties, scanning electron microscope

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Authors: Patricia Mikchaela D. L. Feliciano, Ciela Kadeshka A. Fuentes, Bea Trixia B. Gales, Ethel Princess A. Gepulango, Martin R. Hernandez, Elina Andrea S. Lantion, Jhoe Cynder P. Legaspi, Peter F. Quilala, Gina C. Castro

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Propolis is a resin-like material used by bees to fill large gap holes in the beehive. It has been found to possess anti-inflammatory property, which stimulates hair growth in rats by inducing hair keratinocytes proliferation, causing water retention and preventing damage caused by heat, ultraviolet rays, and other microorganisms without abnormalities in hair follicles. The present study aimed to formulate 10% and 30% Propolis Hair Cream for use in enhancing hair properties. Raw propolis sample was tested for heavy metals using Atomic Absorption Spectroscopy; zinc and chromium were found to be present. Likewise, propolis was extracted in a percolator using 70% ethanol and concentrated under vacuum using a rotary evaporator. The propolis extract was analyzed for total flavonoid content. Compatibility of the propolis extract with excipients was evaluated using Differential Scanning Calorimetry (DSC). No significant changes in organoleptic properties, pH and viscosity of the formulated creams were noted after four weeks of storage at 2-8°C, 30°C, and 40°C. The formulated creams were found to be non-irritating based on the Modified Draize Rabbit Test. In vivo efficacy was evaluated based on thickness and tensile strength of hair grown on previously shaved rat skin. Results show that the formulated 30% propolis-based cream had greater hair enhancing properties than the 10% propolis cream, which had a comparable effect with minoxidil.

Keywords: atomic absorption spectroscopy, differential scanning calorimetry (DSC), modified draize rabbit test, propolis

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Authors: Joanna Gerszon, Aleksandra Rodacka

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In the pathogenesis of neurodegenerative diseases such as Alzheimer's disease and Parkinson's disease, protein and peptide aggregation processes play a vital role in contributing to the formation of intracellular and extracellular protein deposits. One of the major components of these deposits is the oxidatively modified glyceraldehyde-3-phosphate dehydrogenase (GAPDH). Therefore, the purpose of this research was to answer the question whether piceatannol, a stilbene derivative, counteracts and/or slows down oxidative stress-induced GAPDH aggregation. The study also aimed to determine if this natural occurring compound prevents unfavorable nuclear translocation of GAPDH in hippocampal cells. The isothermal titration calorimetry (ITC) analysis indicated that one molecule of GAPDH can bind up to 8 molecules of piceatannol (7.3 ± 0.9). As a consequence of piceatannol binding to the enzyme, the loss of activity was observed. Parallel with GAPDH inactivation the changes in zeta potential, and loss of free thiol groups were noted. Nevertheless, the ligand-protein binding does not influence the secondary structure of the GAPDH. Precise molecular docking analysis of the interactions inside the active center allowed to presume that these effects are due to piceatannol ability to assemble a covalent binding with nucleophilic cysteine residue (Cys149) which is directly involved in the catalytic reaction. Molecular docking also showed that simultaneously 11 molecules of ligand can be bound to dehydrogenase. Taking into consideration obtained data, the influence of piceatannol on level of GAPDH aggregation induced by excessive oxidative stress was examined. The applied methods (thioflavin-T binding-dependent fluorescence as well as microscopy methods - transmission electron microscopy, Congo Red staining) revealed that piceatannol significantly diminishes level of GAPDH aggregation. Finally, studies involving cellular model (Western blot analyses of nuclear and cytosolic fractions and confocal microscopy) indicated that piceatannol-GAPDH binding prevents GAPDH from nuclear translocation induced by excessive oxidative stress in hippocampal cells. In consequence, it counteracts cell apoptosis. These studies demonstrate that by binding with GAPDH, piceatannol blocks cysteine residue and counteracts its oxidative modifications, that induce oligomerization and GAPDH aggregation as well as it prevents hippocampal cells from apoptosis by retaining GAPDH in the cytoplasm. All these findings provide a new insight into the role of piceatannol interaction with GAPDH and present a potential therapeutic strategy for some neurological disorders related to GAPDH aggregation. This work was supported by the by National Science Centre, Poland (grant number 2017/25/N/NZ1/02849).

Keywords: glyceraldehyde-3-phosphate dehydrogenase, neurodegenerative disease, neuroprotection, piceatannol, protein aggregation

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Authors: Sanjay K. Behera, Debasish Saha, Paramesh Gadige, Ranjini Bandyopadhyay

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The zero shear viscosity (η₀) of a suspension of hard sphere colloids characterized by a significant polydispersity (≈10%) increases with increase in volume fraction (ϕ) and shows a dramatic increase at ϕ=ϕg with the system entering a colloidal glassy state. Fragility which is the measure of the rapidity of approach of these suspensions towards the glassy state is sensitive to its size polydispersity and stiffness of the particles. Soft poly(N-isopropylacrylamide) (PNIPAM) particles deform in the presence of neighboring particles at volume fraction above the random close packing volume fraction of undeformed monodisperse spheres. Softness, therefore, enhances the packing efficiency of these particles. In this study PNIPAM particles of a nearly constant swelling ratio and with polydispersities varying over a wide range (7.4%-48.9%) are synthesized to study the effects of polydispersity on the dynamics of suspensions of soft PNIPAM colloidal particles. The size and polydispersity of these particles are characterized using dynamic light scattering (DLS) and scanning electron microscopy (SEM). As these particles are deformable, their packing in aqueous suspensions is quantified in terms of effective volume fraction (ϕeff). The zero shear viscosity (η₀) data of these colloidal suspensions, estimated from rheometric experiments as a function of the effective volume fraction ϕeff of the suspensions, increases with increase in ϕeff and shows a dramatic increase at ϕeff = ϕ₀. The data for η₀ as a function of ϕeff fits well to the Vogel-Fulcher-Tammann equation. It is observed that increasing polydispersity results in increasingly fragile supercooled liquid-like behavior, with the parameter ϕ₀, extracted from the fits to the VFT equation shifting towards higher ϕeff. The observed increase in fragility is attributed to the prevalence of dynamical heterogeneities (DHs) in these polydisperse suspensions, while the simultaneous shift in ϕ₀ is ascribed to the decoupling of the dynamics of the smallest and largest particles. Finally, it is observed that the intrinsic nonlinearity of these suspensions, estimated at the third harmonic near ϕ₀ in Fourier transform oscillatory rheological experiments, increases with increase in polydispersity. These results are in agreement with theoretical predictions and simulation results for polydisperse hard sphere colloidal glasses and clearly demonstrate that jammed suspensions of polydisperse colloidal particles can be effectively fluidized with increasing polydispersity. Suspensions of these particles are therefore excellent candidates for detailed experimental studies of the effects of polydispersity on the dynamics of glass formation.

Keywords: dynamical heterogeneity, effective volume fraction, fragility, intrinsic nonlinearity

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Authors: Mohammed Mesrar, Hamza El Malki, Hamza Mesrar

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In this study, ceramics of (1-x)(Na0.5Bi0.5)TiO3 x(K0.5 Bi0.5)TiO3 were synthesized through a conventional calcination process (solid-state method) at 1000°C for 4 hours, with x(%) values ranging from 0.0 to 100. Room temperature XRD patterns confirmed the phase formation of the samples. The Rietveld refinement method was employed to verify the morphotropic phase boundary (MPB) at x(%)=16-20. We investigated the average crystallite size and lattice strain using Scherrer's formula and Williamson-Hall (W-H) analysis. SEM image analyses provided additional evidence of the impact of doping on structural growth under low temperatures. Relaxation time extracted from Z″(f) and M″(f) spectra for x(%) = 0.0, 12, 16, 20, and 30 followed the Arrhenius law, revealing the presence of three distinct relaxation mechanisms with varying activation energies. The shoulder response in M″(f) indirectly indicated the existence of highly polarizable entities in the samples, serving as a signature of polar nanoregions (PNRs) within the grains.In this study, ceramics of (1-x)(Na0.5Bi0.5)TiO3 x(K0.5 Bi0.5)TiO3 were synthesized through a conventional calcination process (solid-state method) at 1000°C for 4 hours, with x(%) values ranging from 0.0 to 100. Room temperature XRD patterns confirmed the phase formation of the samples. The Rietveld refinement method was employed to verify the morphotropic phase boundary (MPB) at x(%)=16-20. We investigated the average crystallite size and lattice strain using Scherrer's formula and Williamson-Hall (W-H) analysis. SEM image analyses provided additional evidence of the impact of doping on structural growth under low temperatures. Relaxation time extracted from Z″(f) and M″(f) spectra for x(%) = 0.0, 12, 16, 20, and 30 followed the Arrhenius law, revealing the presence of three distinct relaxation mechanisms with varying activation energies. The shoulder response in M″(f) indirectly indicated the existence of highly polarizable entities in the samples, serving as a signature of polar nanoregions (PNRs) within the grains.

Keywords: (1-x)(Na0.5Bi0.5)TiO3 x(K0.5 Bi0.5)TiO3, Rietveld refinement, Scanning electron microscopy (SEM), Williamson-Hall plots, charge density distribution, dielectric properties

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Authors: Faraj M. Elkhatri, Hana Ali Alafi

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The spatial and temporal distribution of diagenetic alterations related impact on the reservoir quality of the Sarir Formation. (present-day burial depth of about 9000 feet) Depositional facies and diagenetic alterations are the main controls on reservoir quality of Sarir Formation Sirt Basin Libya; these based on lithology and grain size as well as authigenic clay mineral types and their distributions. However, petrology investigation obtained on study area with five sandstone wells concentrated on main rock components and the parameters that may have impacts on reservoirs. the main authigenic clay minerals are kaolinite and dickite, these investigations have confirmed by X.R.D analysis and clay fraction. mainly Kaolinite and Dickite were extensively presented on all of wells with high amounts. As well as trace of detrital smectite and less amounts of illitized mud-matrix are possibly found by SEM image. Thin layers of clay presented as clay-grain coatings in local depth interpreted as remains of dissolved clay matrix is partly transformed into kaolinite adjacent and towards pore throat. This also may have impacts on most of the pore throats of this sandstone which are open and relatively clean with some of fine martial have been formed on occluded pores. This material is identified by EDS analysis to be collections of not only kaolinite booklets but also small disaggregated kaolinite platelets derived from the disaggregation of larger kaolinite booklets. These patches of kaolinite not only fill this pore, but also coat some of the surrounding framework grains. Quartz grains often enlarged by authigenic quartz overgrowths partially occlude and reduce porosity. Scanning Electron Microscopy with Energy Dispersive Spectroscopy (SEM) was conducted on the post-test samples to examine any mud filtrate particles that may be in the pore throats. Semi-qualitative elemental data on selected minerals observed during the SEM study were obtained through the use of an Energy Dispersive Spectroscopy (EDS) unit. The samples showed mostly clean open pore throats, with limited occlusion by kaolinite. very fine-grained elemental combinations (Si/Al/Na/Cl, Si/Al Ca/Cl/Ti, and Qtz/Ti) have been identified and conformed by EDS analysis. However, the identification of the fine grained disaggregated material as mainly kaolinite though study area.

Keywords: fine migration, formation damage, kaolinite, soled bulging.

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Authors: Nayeli Camacho, Fernanda Lara-Perez, Carolina Ortega-Portilla, Diego G. Espinosa-Arbelaez, Juan M. Alvarado-Orozco, Guillermo C. Mondragon-Rodriguez

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Ultra-high molecular weight polyethylene (UHMWPE) has been the gold standard material for total knee replacements for almost five decades. Wear damage to UHMWPE articulating surface is inevitable due to the natural sliding and rolling movements of the knee. This generates a considerable amount of wear debris, which results in mechanical instability of the joint, reduces joint mobility, increases pain with detrimental biologic responses, and causes component loosening. The presence of wear particles has been closely related to adverse reactions in the knee joint surrounding tissue, especially for particles in the range of 0.3 to 2 μm. Carbon-based materials possess excellent mechanical properties and have shown great promise in tribological applications. In this study, diamond-like carbon coatings (DLC) and carbon nanotubes (CNTs) were used to decrease the wear rate of ultra-high molecular weight polyethylene. A titanium doped DLC (Ti-DLC) was deposited by magnetron sputtering on stainless steel precision spheres while CNTs were used as a second phase reinforcement in UHMWPE at a concentration of 1.25 wt.%. A comparative tribological analysis of the wear of UHMWPE and UHMWPE-CNTs with a stainless steel counterpart with and without Ti-DLC coating is presented. The experimental wear testing was performed on a pin-on-disc tribometer under dry conditions, using a reciprocating movement with a load of 1 N at a frequency of 2 Hz for 100,000 and 200,000 cycles. The wear tracks were analyzed with high-resolution scanning electron microscopy to determine wear modes and observe the size and shape of the wear debris. Furthermore, profilometry was used to study the depth of the wear tracks and to map the wear of the articulating surface. The wear tracks at 100,000 and 200,000 cycles on all samples were relatively shallow, and they were in the range of average roughness. It was observed that the Ti-DLC coating decreases the mass loss in the UHMWPE and the depth of the wear track. The combination of both carbon-based materials decreased the material loss compared to the system of stainless steel and UHMWPE. Burnishing of the surface was the predominant wear mode observed with all the systems, more subtle for the systems with Ti-DLC coatings. Meanwhile, in the system composed of stainless steel-UHMWPE, the intrinsic surface roughness of the material was completely replaced by the wear tracks.

Keywords: CNT reinforcement, self-lubricating materials, Ti-DLC, UHMWPE tribological performance

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