Search results for: immuno-transmission electron microscopy

Authors: D. Bikiaris, M. Nerantzaki, I. Koliakou, A. Francone, N. Kehagias

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In the present study, the formation of structures in poly(lactic acid) (PLA) has been investigated with respect to producing areas of regular, superficial features with dimensions comparable to those of cells or biological macromolecules. Nanoimprint lithography, a method of pattern replication in polymers, has been used for the production of features ranging from tens of micrometers, covering areas up to 1 cm², down to hundreds of nanometers. Both micro- and nano-structures were faithfully replicated. Potentially, PLA has wide uses within biomedical fields, from implantable medical devices, including screws and pins, to membrane applications, such as wound covers, and even as an injectable polymer for, for example, lipoatrophy. The possibility of fabricating structured PLA surfaces, with structures of the dimensions associated with cells or biological macro- molecules, is of interest in fields such as cellular engineering. Imprint-based technologies have demonstrated the ability to selectively imprint polymer films over large areas resulting in 3D imprints over flat, curved or pre-patterned surfaces. Here, we compare nano-patterned with nano-patterned by nanoimprint lithography (NIL) PLA film. A silicon nanostructured stamp (provided by Nanotypos company) having positive and negative protrusions was used to pattern PLA films by means of thermal NIL. The polymer film was heated from 40°C to 60°C above its Tg and embossed with a pressure of 60 bars for 3 min. The stamp and substrate were demolded at room temperature. Scanning electron microscope (SEM) images showed good replication fidelity of the replicated Si stamp. Contact-angle measurements suggested that positive microstructuring of the polymer (where features protrude from the polymer surface) produced a more hydrophilic surface than negative micro-structuring. The ability to structure the surface of the poly(lactic acid), allied to the polymer’s post-processing transparency and proven biocompatibility. Films produced in this were also shown to enhance the aligned attachment behavior and proliferation of Wharton’s Jelly Mesenchymal Stem cells, leading to the observed growth contact guidance. The bacterial attachment patterns of some bacteria, highlighted that the nano-patterned PLA structure can reduce the propensity for the bacteria to attach to the surface, with a greater bactericidal being demonstrated activity against the Staphylococcus aureus cells. These biocompatible, micro- and nanopatterned PLA surfaces could be useful for polymer– cell interaction experiments at dimensions at, or below, that of individual cells. Indeed, post-fabrication modification of the microstructured PLA surface, with materials such as collagen (which can further reduce the hydrophobicity of the surface), will extend the range of applications, possibly through the use of PLA’s inherent biodegradability. Further study is being undertaken to examine whether these structures promote cell growth on the polymer surface.

Keywords: poly(lactic acid), nano-imprint lithography, anti-bacterial properties, PLA

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Authors: Suman Chaudhary, Rupinder K. Kanwar, Jagat R. Kanwar

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Azadirachta indica, also known as Neem belonging to the mahogany family is actively gaining interest in the era of modern day medicine due to its extensive applications in homeopathic medicine such as Ayurveda and Unani. More than 140 phytochemicals have been extracted from neem leaves, seed, bark and flowers for agro-medicinal applications. Among the various components, neem leaf protein (NLP) is currently the most investigated active ingredient, due to its immunomodulatory activities against tumor growth. However, these therapeutic ingredients of neem are susceptible to degradation and cannot withstand the drastic pH changes under physiological environment, and therefore, there is an urgent need of an alternative strategy such as a nano-delivery system to exploit its medicinal benefits. This study hypothesizes that guar gum (GG) derived biodegradable nano-carrier based encapsulation of NLP will improve its stability, specificity and sensitivity, thus facilitating targeted anti-cancer therapeutics. GG is a galactomannan derived from the endosperm of the guar beans seeds. Synthesis of guar nanocapsules (NCs) was performed using nanoprecipitation technique where the GG was encapsulated with NLP. Preliminary experiments conducted to characterize the NCs confirmed spherical morphology with a narrow size distribution of 30-40 nm. Differential scanning colorimetric analysis (DSC) validated the stability of these NCs even at a temperature range of 50-60°C which was well within the physiological and storage conditions. Thermogravimetric (TGA) analysis indicated high decomposition temperature of these NCs ranging upto 350°C. Additionally, Fourier Transform Infrared spectroscopy (FTIR) and the SDS-PAGE data acquired confirmed the successful encapsulation of NLP in the NCs. The anti-cancerous therapeutic property of this NC was tested on colon cancer cells (caco-2) as they are one of the most prevalent form of cancer. These NCs (both NLP loaded and void) were also tested on human intestinal epithelial cells (FHs 74) cells to evaluate their effect on normal cells. Cytotoxicity evaluation of the NCs in the cell lines confirmed that the IC50 for NLP in FHs 74 cells was ~2 fold higher than in caco-2 cells, indicating that this nanoformulation system possessed biocompatible anti-cancerous properties Immunoconfocal microscopy analysis confirmed the time dependent internalization of the NCs within 6h. Recent findings performed using Annexin V and PI staining indicated a significant increase (p ≤ 0.001) in the early and late apoptotic cell population when treated with the NCs signifying the role of NLP in inducing apoptosis in caco-2 cells. This was further validated using Western blot, Polymerase chain reaction (PCR) and Fluorescence activated cell sorter (FACS) aided protein expressional analysis which presented a downregulation of survivin, an anti-apoptotic cell marker and upregulation of Bax/Bcl-2 ratio (pro-apoptotic indicator). Further, both the NLP NC and unencapsulated NLP treatment destabilized the mitochondrial membrane potential subsequently facilitating the release of the pro-apoptotic caspase cascade initiator, cytochrome-c. Future studies will be focused towards granting specificity to these NCs towards cancer cells, along with a comprehensive analysis of the anti-cancer potential of this naturally occurring compound in different cancer and in vivo animal models, will validate the clinical application of this unprecedented protein therapeutic.

Keywords: anti-tumor, guar gum, nanocapsules, neem leaf protein

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Authors: Serdar Delice, Mehmet Isik, Nizami Hasanli, Kadir Goksen

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Researchers have donated great interest to ternary and quaternary semiconductor compounds especially with the improvement of the optoelectronic technology. The quaternary compound Tl2Ga2Se3S which was grown by Bridgman method carries the properties of ternary thallium chalcogenides group of semiconductors with layered structure. This compound can be formed from TlGaSe2 crystals replacing the one quarter of selenium atom by sulfur atom. Although Tl2Ga2Se3S crystals are not intentionally doped, some unintended defect types such as point defects, dislocations and stacking faults can occur during growth processes of crystals. These defects can cause undesirable problems in semiconductor materials especially produced for optoelectronic technology. Defects of various types in the semiconductor devices like LEDs and field effect transistor may act as a non-radiative or scattering center in electron transport. Also, quick recombination of holes with electrons without any energy transfer between charge carriers can occur due to the existence of defects. Therefore, the characterization of defects may help the researchers working in this field to produce high quality devices. Thermoluminescence (TL) is an effective experimental method to determine the kinetic parameters of trap centers due to defects in crystals. In this method, the sample is illuminated at low temperature by a light whose energy is bigger than the band gap of studied sample. Thus, charge carriers in the valence band are excited to delocalized band. Then, the charge carriers excited into conduction band are trapped. The trapped charge carriers are released by heating the sample gradually and these carriers then recombine with the opposite carriers at the recombination center. By this way, some luminescence is emitted from the samples. The emitted luminescence is converted to pulses by using an experimental setup controlled by computer program and TL spectrum is obtained. Defect characterization of Tl2Ga2Se3S single crystals has been performed by TL measurements at low temperatures between 10 and 300 K with various heating rate ranging from 0.6 to 1.0 K/s. The TL signal due to the luminescence from trap centers revealed one glow peak having maximum temperature of 36 K. Curve fitting and various heating rate methods were used for the analysis of the glow curve. The activation energy of 13 meV was found by the application of curve fitting method. This practical method established also that the trap center exhibits the characteristics of mixed (general) kinetic order. In addition, various heating rate analysis gave a compatible result (13 meV) with curve fitting as the temperature lag effect was taken into consideration. Since the studied crystals were not intentionally doped, these centers are thought to originate from stacking faults, which are quite possible in Tl2Ga2Se3S due to the weakness of the van der Waals forces between the layers. Distribution of traps was also investigated using an experimental method. A quasi-continuous distribution was attributed to the determined trap centers.

Keywords: chalcogenides, defects, thermoluminescence, trap centers

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Authors: K. J. Sannapapamma, H. Malligawad Lokanath, Sakeena Naikwadi

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Eco-friendly textiles are gaining importance among the consumers and textile manufacturers in the healthcare sector due to increased environmental pollution which leads to several health and environmental hazards. Hence, the research was designed to cultivate and develop the organic cotton knit, to prepare and characterize the Vetiver oil microcapsules for textile finishing and to access the wash durability of finished knits. The cotton SAHANA variety grown under organic production systems was processed and spun into 30 single yarn dyed with four natural colorants (Arecanut slurry, Eucalyptus leaves, Pomegranate rind and Indigo) and eco dyed yarn was further used for development of single jersy knitted fabric. Vetiveria zizanioides is an aromatic grass which is being traditionally used in medicine and perfumery. Vetiver essential oil was used for preparation of microcapsules by interfacial polymerization technique subjected to Gas Chromatography Mass Spectrometry (GCMS), Fourier Transform Infrared Spectroscopy (FTIR), Thermo Gravimetric Analyzer (TGA) and Scanning Electron Microscope (SEM) for characterization of microcapsules. The knitted fabric was finished with vetiver oil microcapsules by exhaust and pad dry cure methods. The finished organic knit was assessed for laundering on antimicrobial efficiency and aroma intensity. GCMS spectral analysis showed that, diethyl phthalate (28%) was the major compound found in vetiver oil followed by isoaromadendrene epoxide (7.72%), beta-vetivenene (6.92%), solavetivone (5.58%), aromadenderene, azulene and khusimol. Bioassay explained that, the vetiver oil and diluted vetiver oil possessed greater zone of inhibition against S. aureus and E. coli than the coconut oil. FTRI spectra of vetiver oil and microcapsules possessed similar peaks viz., C-H, C=C & C꞊O stretching and additionally oil microcapsules possessed the peak of 3331.24 cm^-1 at 91.14 transmittance was attributed to N-H stretches. TGA of oil microcapsules revealed that, there was a minimum weight loss (5.835%) recorded at 467.09°C compared to vetiver oil i.e., -3.026% at the temperature of 396.24°C. The shape of the microcapsules was regular and round, some were spherical in shape and few were rounded by small aggregates. Irrespective of methods of application, organic cotton knits finished with microcapsules by pad dry cure method showed maximum zone of inhibition compared to knits finished by exhaust method against S. aureus and E. coli. The antimicrobial activity of the finished samples was subjected to multiple washing which indicated that knits finished with pad dry cure method showed a zone of inhibition even after 20^th wash and better aroma retention compared to knits finished with the exhaust method of application. Further, the group of respondents rated that the 5^th washed samples had the greater aroma intensity in both the methods than the other samples. Thus, the vetiver microencapsulated organic cotton knits are free from hazardous chemicals and have multi-functional properties that can be suitable for medical and healthcare textiles.

Keywords: exhaust and pad dry cure finishing, interfacial polymerization, organic cotton knits, vetiver oil microcapsules

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Authors: Animesh Pan, Geoffrey D. Bothun

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With the development of nanotechnology, research in multifunctional delivery systems has a new pace and dimension. An incipient challenge is to design an all-in-one delivery system that can be used for multiple purposes, including tumor targeting therapy, radio-frequency (RF-), near-infrared (NIR-), light-, or pH-induced controlled release, photothermal therapy (PTT), photodynamic therapy (PDT), and medical diagnosis. In this regard, various inorganic nanoparticles (NPs) are known to show great potential as the 'functional components' because of their fascinating and tunable physicochemical properties and the possibility of multiple theranostic modalities from individual NPs. Magnetic, luminescent, and plasmonic properties are the three most extensively studied and, more importantly biomedically exploitable properties of inorganic NPs. Although successful attempts of combining any two of them above mentioned functionalities have been made, integrating them in one system has remained challenge. Keeping those in mind, controlled designs of complex colloidal nanoparticle system are one of the most significant challenges in nanoscience and nanotechnology. Therefore, systematic and planned studies providing better revelation are demanded. We report a multifunctional delivery platform-based liposome loaded with drug, iron-oxide magnetic nanoparticles (MNPs), and a gold shell on the surface of liposomes, were synthesized using a lipid with polyelectrolyte (layersomes) templating technique. MNPs and the anti-cancer drug doxorubicin (DOX) were co-encapsulated inside liposomes composed by zwitterionic phophatidylcholine and anionic phosphatidylglycerol using reverse phase evaporation (REV) method. The liposomes were coated with positively charge polyelectrolyte (poly-L-lysine) to enrich the interface with gold anion, exposed to a reducing agent to form a gold nanoshell, and then capped with thio-terminated polyethylene glycol (SH-PEG2000). The core-shell nanostructures were characterized by different techniques like; UV-Vis/NIR scanning spectrophotometer, dynamic light scattering (DLS), transmission electron microscope (TEM). This multifunctional system achieves a variety of functions, such as radiofrequency (RF)-triggered release, chemo-hyperthermia, and NIR laser-triggered for photothermal therapy. Herein, we highlight some of the remaining major design challenges in combination with preliminary studies assessing therapeutic objectives. We demonstrate an efficient loading and delivery system to significant cell death of human cancer cells (A549) with therapeutic capabilities. Coupled with RF and NIR excitation to the doxorubicin-loaded core-shell nanostructure helped in securing targeted and controlled drug release to the cancer cells. The present core-shell multifunctional system with their multimodal imaging and therapeutic capabilities would be eminent candidates for cancer theranostics.

Keywords: cancer thernostics, multifunctional nanostructure, photothermal therapy, radiofrequency targeting

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Authors: Nikola Toshikj, Michel Ramonda, Sylvain Catrouillet, Jean-Jacques Robin, Sebastien Blanquer

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Biodegradable and biocompatible block copolymers have risen as the golden materials in both medical and environmental applications. Moreover, if their architecture is of controlled manner, higher applications can be foreseen. In the meantime, organocatalytic ROP has been promoted as more rapid and immaculate route, compared to the traditional organometallic catalysis, towards efficient synthesis of block copolymer architectures. Therefore, herein we report novel organocatalytic pathway with guanidine molecules (TBD) for supported synthesis of trimethylene carbonate initiated by poly(caprolactone) as pre-polymer. Pristine PTMC-b-PCL-b-PTMC block copolymer structure, without any residual products and clear desired block proportions, was achieved under 1.5 hours at room temperature and verified by NMR spectroscopies and size-exclusion chromatography. Besides, when elaborating block copolymer films, further stability and amelioration of mechanical properties can be achieved via additional reticulation step of precedently methacrylated block copolymers. Subsequently, stimulated by the insufficient studies on the phase-separation/crystallinity relationship in these semi-crystalline block copolymer systems, their intrinsic thermal and morphology properties were investigated by differential scanning calorimetry and atomic force microscopy. Firstly, by DSC measurements, the block copolymers with χABN values superior to 20 presented two distinct glass transition temperatures, close to the ones of the respecting homopolymers, demonstrating an initial indication of a phase-separated system. In the interim, the existence of the crystalline phase was supported by the presence of melting temperature. As expected, the crystallinity driven phase-separated morphology predominated in the AFM analysis of the block copolymers. Neither crosslinking at melted state, hence creation of a dense polymer network, disturbed the crystallinity phenomena. However, the later revealed as sensible to rapid liquid nitrogen quenching directly from the melted state. Therefore, AFM analysis of liquid nitrogen quenched and crosslinked block copolymer films demonstrated a thermodynamically driven phase-separation clearly predominating over the originally crystalline one. These AFM films remained stable with their morphology unchanged even after 4 months at room temperature. However, as demonstrated by DSC analysis once rising the temperature above the melting temperature of the PCL block, neither the crosslinking nor the liquid nitrogen quenching shattered the semi-crystalline network, while the access to thermodynamical phase-separated structures was possible for temperatures under the poly (caprolactone) melting point. Precisely this coexistence of dual crosslinked/crystalline networks in the same copolymer structure allowed us to establish, for the first time, the shape-memory properties in such materials, as verified by thermomechanical analysis. Moreover, the response temperature to the material original shape depended on the block copolymer emplacement, hence PTMC or PCL as end-block. Therefore, it has been possible to reach a block copolymer with transition temperature around 40°C thus opening potential real-life medical applications. In conclusion, the initial study of phase-separation/crystallinity relationship in PTMC-b-PCL-b-PTMC block copolymers lead to the discovery of novel shape memory materials with superior properties, widely demanded in modern-life applications.

Keywords: biodegradable block copolymers, organocatalytic ROP, self-assembly, shape-memory

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Authors: Magdalena Maria Rost-Roszkowska, Alina Chachulska-Żymełka, Monika Tarnawska, Maria Augustyniak, Alina Kafel, Agnieszka Babczyńska

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The digestive system of insects is composed of three distinct regions: fore-, mid- and hingut. The middle region (the midgut) is treated as one of the barriers which protects the organism against any stressors which originate from external environment, e.g. toxic metals. Such factors can activate the cell death in epithelial cells to preserve the entire tissue/organs against the degeneration. Different mechanisms involved in homeostasis maintenance have been described, but the studies of animals under field conditions do not give the opportunity to conclude about potential ability of subsequent generation to inherit the tolerance mechanisms. It is possible only by a multigenerational strain of an animal led under laboratory conditions, exposed to a selected toxic factor, present also in polluted ecosystems. The main purpose of the project was to check if changes, which appear in the midgut epithelium after Cd treatment, can be fixed during the following generations of insects with the special emphasis on apoptosis. As the animal for these studies we chose 5th larval stage of the beet armyworm Spodoptera exigua Hübner (Lepidoptera: Noctuidae), which is one of pest of many vegetable crops. Animals were divided into some experimental groups: K, Cd, KCd, Cd1, Cd2, Cd3. A control group (K) fed a standard diet, and was conducted for XX generations, a cadmium group (Cd), fed on standard diet supplemented with cadmium (44 mg Cd per kg of dry weight of food) for XXX generations. A reference Cd group (KCd) has been initiated: control insects were fed with Cd supplemented diet (44 mg Cd per kg of dry weight of food). Experimental groups Cd1, Cd2, Cd3 developed from the control one: 5 mg Cd per kg of dry weight of food, 10 mg Cd per kg of dry weight of food, 20 mg Cd per kg of dry weight of food. We were interested in the activation of apoptosis during following generations in all experimental groups. Therefore, during the 1st year of the experiment, the measurements were done for 6 generations in all experimental group. The intensity and the course of apoptosis have been examined using transmission electron microscope (TEM), confocal microscope and flow cytometry. During apoptosis the cell started to shrink, extracellular spaces appeared between digestive and neighboring cells, the nucleus achieved a lobular shape. Eventually, the apoptotic cells was discharged into the midgut lumen. A quantitative analysis revealed that the number of apoptotic cells depends significantly on the generation, tissue and cadmium concentration in the insect rearing medium. In the following 6 generations, we observed that the percentage of apoptotic cells in the midguts from cadmium-exposed groups decreased gradually according to the following order of strains: Cd1, Cd2, Cd3 and KCd. At the same time, it was still higher than the percentage of apoptotic cells in the same tissues of the insects from the control and multigenerational cadmium strain. The results of our studies suggest that changes caused by cadmium treatment were preserved during 6-generational development of lepidopteran larvae. The study has been financed by the National Science Centre Poland, grant no 2016/21/B/NZ8/00831.

Keywords: cadmium, cell death, digestive system, ultrastructure

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Authors: Jessie Rapoza, Petr Moroshkin, Jimmy Xu

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Chirality is omnipresent, in nature, in life, and in the field of physics. One intriguing example is the homochirality that has remained a great secret of life. Another is the pairs of mirror-image molecules – enantiomers. They are identical in atomic composition and therefore indistinguishable in the scalar physical properties. Yet, they can be either therapeutic or toxic, depending on their chirality. Recent studies suggest a potential link between abnormal levels of certain D-amino acids and some serious health impairments, including schizophrenia, amyotrophic lateral sclerosis, and potentially cancer. Although indistinguishable in their scalar properties, the chirality of a molecule reveals itself in interaction with the surrounding of a certain chirality, or more generally, a broken mirror-symmetry. In this work, we report on a system for chiral molecule detection, in which the mirror-symmetry is doubly broken, first by asymmetric structuring a nanopatterned plasmonic surface than by the incidence of circularly polarized light (CPL). In this system, the incident circularly-polarized light induces a surface plasmon polariton (SPP) wave, propagating along the asymmetric plasmonic surface. This SPP field itself is chiral, evanescently bound to a near-field zone on the surface (~10nm thick), but with an amplitude greatly intensified (by up to 104) over that of the incident light. It hence probes just the molecules on the surface instead of those in the volume. In coupling to molecules along its path on the surface, the chiral SPP wave favors one chirality over the other, allowing for chirality detection via the change in an optical rectification current measured at the edges of the sample. The asymmetrically structured surface converts the high-frequency electron plasmonic-oscillations in the SPP wave into a net DC drift current that can be measured at the edge of the sample via the mechanism of optical rectification. The measured results validate these design concepts and principles. The observed optical rectification current exhibits a clear differentiation between a pair of enantiomers. Experiments were performed by focusing a 1064nm CW laser light at the sample - a gold grating microchip submerged in an approximately 1.82M solution of either L-arabinose or D-arabinose and water. A measurement of the current output was then recorded under both rights and left circularly polarized lights. Measurements were recorded at various angles of incidence to optimize the coupling between the spin-momentums of the incident light and that of the SPP, that is, spin-momentum locking. In order to suppress the background, the values of the photocurrent for the right CPL are subtracted from those for the left CPL. Comparison between the two arabinose enantiomers reveals a preferential signal response of one enantiomer to left CPL and the other enantiomer to right CPL. In sum, this work reports on the first experimental evidence of the feasibility of chiral molecule detection via optical rectification in a metal meta-grating. This nanoscale interfaced electrical detection technology is advantageous over other detection methods due to its size, cost, ease of use, and integration ability with read-out electronic circuits for data processing and interpretation.

Keywords: Chirality, detection, molecule, spin

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Authors: Kyoung Lee

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Numerous aerobic bacteria have the ability to form multicellular communities on the surface layer of the air-liquid (A-L) interface as a biofilm called a pellicle. Pellicles occupied at the A-L interface will benefit from the utilization of oxygen from air and nutrient from liquid. Buoyancy of cells can be obtained by high surface tension at the A-L interface. Thus, formation of pellicles is an adaptive advantage in utilization of excess nutrients in the standing culture where oxygen depletion is easily set up due to rapid cell growth. In natural environments, pellicles are commonly observed on the surface of lake or pond contaminated with pollutants. Previously, we have shown that when cultured in standing LB media an alkylphenol-degrading bacteria Pseudomonas alkylphenolia KL28 forms pellicles in a diameter of 0.3-0.5 mm with a thickness of ca 40 µm. The pellicles have unique features for possessing flatness and unusual rigidity. In this study, the biogenesis of the circular pellicles has been investigated by observing the cell organization at early stages of pellicle formation and cell arrangements in pellicle, providing a clue for highly organized cellular arrangement to be adapted to the air-liquid niche. Here, we first monitored developmental patterns of pellicle from monolayer to multicellular organization. Pellicles were shaped by controlled growth of constituent cells which accumulate extracellular polymeric substance. The initial two-dimensional growth was transited to multilayers by a constraint force of accumulated self-produced extracellular polymeric substance. Experiments showed that pellicles are formed by clonal growth and even with knock-out of genes for flagella and pilus formation. In contrast, the mutants in the epm gene cluster for alginate-like polymer biosynthesis were incompetent in cell alignment for initial two-dimensional growth of pellicles. Electron microscopic and confocal laser scanning microscopic studies showed that the fully matured structures are highly packed by matrix-encased cells which have special arrangements. The cells on the surface of the pellicle lie relatively flat and inside longitudinally cross packed. HPLC analysis of the extrapolysaccharide (EPS) hydrolysate from the colonies from LB agar showed a composition with L-fucose, L-rhamnose, D-galactosamine, D-glucosamine, D-galactose, D-glucose, D-mannose. However, that from pellicles showed similar neutral and amino sugar profile but missing galactose. Furthermore, uronic acid analysis of EPS hydrolysates by HPLC showed that mannuronic acid was detected from pellicles not from colonies, indicating the epm-derived polymer is critical for pellicle formation as proved by the epm mutants. This study verified that for the circular pellicle architecture P. alkylphenolica KL28 cells utilized EPS building blocks different from that used for colony construction. These results indicate that P. alkylphenolica KL28 is a clever architect that dictates unique cell arrangements with selected EPS matrix material to construct sophisticated building, circular biofilm pellicles.

Keywords: biofilm, matrix, pellicle, pseudomonas

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Authors: Guoheng Liu, Zhilong Huang

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For more than the past ten years, oil and gas production from marine shale such as the Barnett shale. In addition, in recent years, major breakthroughs have also been made in lacustrine shale gas exploration, such as the Yanchang Formation of the Ordos Basin in China. Lucaogou Formation shale, which is also lacustrine shale, has also yielded a high production in recent years, for wells such as M1, M6, and ML2, yielding a daily oil production of 5.6 tons, 37.4 tons and 13.56 tons, respectively. Lithologic identification and classification of reservoirs are the base and keys to oil and gas exploration. Lithology and lithofacies obviously control the distribution of oil and gas in lithological reservoirs, so it is of great significance to describe characteristics of lithology and lithofacies of reservoirs finely. Lithofacies is an intrinsic property of rock formed under certain conditions of sedimentation. Fine-grained sedimentary rocks such as shale formed under different sedimentary conditions display great particularity and distinctiveness. Hence, to our best knowledge, no constant and unified criteria and methods exist for fine-grained sedimentary rocks regarding lithofacies definition and classification. Consequently, multi-parameters and multi-disciplines are necessary. A series of qualitative descriptions and quantitative analysis were used to figure out the lithofacies characteristics and its effect on oil accumulation of Lucaogou formation fine-grained sedimentary rocks in Santanghu basin. The qualitative description includes core description, petrographic thin section observation, fluorescent thin-section observation, cathode luminescence observation and scanning electron microscope observation. The quantitative analyses include X-ray diffraction, total organic content analysis, ROCK-EVAL.II Methodology, soxhlet extraction, porosity and permeability analysis and oil saturation analysis. Three types of lithofacies were mainly well-developed in this study area, which is organic-rich massive shale lithofacies, organic-rich laminated and cloddy hybrid sedimentary lithofacies and organic-lean massive carbonate lithofacies. Organic-rich massive shale lithofacies mainly include massive shale and tuffaceous shale, of which quartz and clay minerals are the major components. Organic-rich laminated and cloddy hybrid sedimentary lithofacies contain lamina and cloddy structure. Rocks from this lithofacies chiefly consist of dolomite and quartz. Organic-lean massive carbonate lithofacies mainly contains massive bedding fine-grained carbonate rocks, of which fine-grained dolomite accounts for the main part. Organic-rich massive shale lithofacies contain the highest content of free hydrocarbon and solid organic matter. Moreover, more pores were developed in organic-rich massive shale lithofacies. Organic-lean massive carbonate lithofacies contain the lowest content solid organic matter and develop the least amount of pores. Organic-rich laminated and cloddy hybrid sedimentary lithofacies develop the largest number of cracks and fractures. To sum up, organic-rich massive shale lithofacies is the most favorable type of lithofacies. Organic-lean massive carbonate lithofacies is impossible for large scale oil accumulation.

Keywords: lithofacies classification, tuffaceous shale, oil enrichment, Lucaogou formation

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Authors: Eduardo Martínez González, Mousumi Dey, Pekka Peljo

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Transitioning to a renewable energy model is inevitable owing to the effects of climate change. These energies are aimed at sustainability and a positive impact on the environment, but they are intermittent energies; their connection to the electrical grid depends on creating long-term, efficient, and low-cost energy storage devices. Redox flow batteries are attractive technologies to address this problem, as they store energy in solution through external tanks known as posolyte (solution to storage positive charge) and negolyte (solution to storage negative charge). During the charging process of the device, the posolyte and negolyte solutions are pumped into an electrochemical cell (which has the anode and cathode separated by an ionic membrane), where they undergo oxidation and reduction reactions at electrodes, respectively. The electrogenerated species should be stable and diffuse into the bulk solution. It has been possible to connect gigantic redox flow batteries to the electrical grid. However, the devices created do not fit with the sustainability criteria since their electroactive material consists of vanadium (material scarce and expensive) solutions dissolved in an acidic medium (e.g., 9 mol L-1 of H₂SO₄) that is highly corrosive; so, work is being done on the design of organic-electroactive electrolytes (posolytes and nogolytes) for their operation at different pH values, including neutral medium. As a main characteristic, negolyte species should have low reduction potential values, while the reverse is true for the oxidation process of posolytes. A wide variety of negolytes that store 1 and up to 2 electrons per molecule (in aqueous medium) have been publised. Gallocyanine compound was recently introduced as an electroactive material for developing alkaline flow battery negolytes. The system can storage two electrons per molecule, but its unexpectedly low water solubility was improved with an amino sulphonic acid additive. The cycling stability of and improved gallocyanine electrolyte was demonstrated by operating a flow battery cell (pairing the system to a posolyte composed of ferri/ferrocyanide solution) outside a glovebox. We also discovered that the additive improves the solubility of gallocyanine, but there is a kinetic price to pay for this advantage. Therefore, in this work, the effect of different amino sulphonic acid derivatives on the kinetics and solubility of gallocyanine compound was studied at alkaline solutions. The additive providing a faster electron transfer rate and high solubility was tested in a flow battery cell. An aqueous organic flow battery electrolyte working outside a glovebox with 15 mAhL-1 will be discussed. Acknowledgments: To Bi3BoostFlowBat Project (2021-2025), funded by the European Research Concil. For support with infrastructure, reagents, and a postdoctoral fellowship to Dr. Martínez-González.

Keywords: alkaline flow battery, gallocyanine electroactive material, amine-sulphonic acid additives, improved solubility

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Authors: Mariia V. Efremova, Iana O. Tcareva, Anastasia D. Blokhina, Ivan S. Grebennikov, Anastasia S. Garanina, Maxim A. Abakumov, Yury I. Golovin, Alexander G. Savchenko, Alexander G. Majouga, Natalya L. Klyachko

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During last decades magnetite nanoparticles (NPs) attract a deep interest of scientists due to their potential application in therapy and diagnostics. However, magnetite nanoparticles are toxic and non-stable in physiological conditions. To solve these problems, we decided to create two types of hybrid systems based on magnetite and gold which is inert and biocompatible: gold as a shell material (first type) and gold as separate NPs interfacially bond to magnetite NPs (second type). The synthesis of the first type hybrid nanoparticles was carried out as follows: Magnetite nanoparticles with an average diameter of 9±2 nm were obtained by co-precipitation of iron (II, III) chlorides then they were covered with gold shell by iterative reduction of hydrogen tetrachloroaurate with hydroxylamine hydrochloride. According to the TEM, ICP MS and EDX data, final nanoparticles had an average diameter of 31±4 nm and contained iron even after hydrochloric acid treatment. However, iron signals (K-line, 7,1 keV) were not localized so we can’t speak about one single magnetic core. Described nanoparticles covered with mercapto-PEG acid were non-toxic for human prostate cancer PC-3/ LNCaP cell lines (more than 90% survived cells as compared to control) and had high R2-relaxivity rates (>190 mМ-1s-1) that exceed the transverse relaxation rate of commercial MRI-contrasting agents. These nanoparticles were also used for chymotrypsin enzyme immobilization. The effect of alternating magnetic field on catalytic properties of chymotrypsin immobilized on magnetite nanoparticles, notably the slowdown of catalyzed reaction at the level of 35-40 % was found. The synthesis of the second type hybrid nanoparticles also involved two steps. Firstly, spherical gold nanoparticles with an average diameter of 9±2 nm were synthesized by the reduction of hydrogen tetrachloroaurate with oleylamine; secondly, they were used as seeds during magnetite synthesis by thermal decomposition of iron pentacarbonyl in octadecene. As a result, so-called dumbbell-like structures were obtained where magnetite (cubes with 25±6 nm diagonal) and gold nanoparticles were connected together pairwise. By HRTEM method (first time for this type of structure) an epitaxial growth of magnetite nanoparticles on gold surface with co-orientation of (111) planes was discovered. These nanoparticles were transferred into water by means of block-copolymer Pluronic F127 then loaded with anti-cancer drug doxorubicin and also PSMA-vector specific for LNCaP cell line. Obtained nanoparticles were found to have moderate toxicity for human prostate cancer cells and got into the intracellular space after 45 minutes of incubation (according to fluorescence microscopy data). These materials are also perspective from MRI point of view (R2-relaxivity rates >70 mМ-1s-1). Thereby, in this work magnetite-gold hybrid nanoparticles, which have a strong potential for biomedical application, particularly in targeted drug delivery and magnetic resonance imaging, were synthesized and characterized. That paves the way to the development of special medicine types – theranostics. The authors knowledge financial support from Ministry of Education and Science of the Russian Federation (14.607.21.0132, RFMEFI60715X0132). This work was also supported by Grant of Ministry of Education and Science of the Russian Federation К1-2014-022, Grant of Russian Scientific Foundation 14-13-00731 and MSU development program 5.13.

Keywords: drug delivery, magnetite-gold, MRI contrast agents, nanoparticles, toxicity

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Authors: Manish Saha, Manish Kumar Niranjan, Saket Asthana

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The K₀.₅Na₀.₅NbO₃ (KNN) system has emerged as one of the most promising lead-free piezoelectric over the years. In this work, we perform a comprehensive investigation of electronic structure, lattice dynamics and dielectric/ferroelectric properties of the room temperature phase of KNN by combining ab-initio DFT-based theoretical analysis and experimental characterization. We assign the symmetry labels to KNN vibrational modes and obtain ab-initio polarized Raman spectra, Infrared (IR) reflectivity, Born-effective charge tensors, oscillator strengths etc. The computed Raman spectrum is found to agree well with the experimental spectrum. In particular, the results suggest that the mode in the range ~840-870 cm-¹ reported in the experimental studies is longitudinal optical (LO) with A_1 symmetry. The Raman mode intensities are calculated for different light polarization set-ups, which suggests the observation of different symmetry modes in different polarization set-ups. The electronic structure of KNN is investigated, and an optical absorption spectrum is obtained. Further, the performances of DFT semi-local, metal-GGA and hybrid exchange-correlations (XC) functionals, in the estimation of KNN band gaps are investigated. The KNN bandgap computed using GGA-1/2 and HSE06 hybrid functional schemes are found to be in excellant agreement with the experimental value. The COHP, electron localization function and Bader charge analysis is also performed to deduce the nature of chemical bonding in the KNN. The solid-state reaction and hydrothermal methods are used to prepare the KNN ceramics, and the effects of grain size on the physical characteristics these ceramics are examined. A comprehensive study on the impact of different synthesis techniques on the structural, electrical, and photocatalytic properties of ferroelectric ceramics KNN. The KNN-S prepared by solid-state method have significantly larger grain size as compared to that for KNN-H prepared by hydrothermal method. Furthermore, the KNN-S is found to exhibit higher dielectric, piezoelectric and ferroelectric properties as compared to KNN-H. On the other hand, the increased photocatalytic activity is observed in KNN-H as compared to KNN-S. As compared to the hydrothermal synthesis, the solid-state synthesis causes an increase in the relative dielectric permittivity (ε^') from 2394 to 3286, remnant polarization (P_r) from 15.38 to 20.41 μC/cm^², planer electromechanical coupling factor (k_p) from 0.19 to 0.28 and piezoelectric coefficient (d_33) from 88 to 125 pC/N. The KNN-S ceramics are also found to have a lower leakage current density, and higher grain resistance than KNN-H ceramic. The enhanced photocatalytic activity of KNN-H is attributed to relatively smaller particle sizes. The KNN-S and KNN-H samples are found to have degradation efficiencies of RhB solution of 20% and 65%, respectively. The experimental study highlights the importance of synthesis methods and how these can be exploited to tailor the dielectric, piezoelectric and photocatalytic properties of KNN. Overall, our study provides several bench-mark important results on KNN that have not been reported so far.

Keywords: lead-free piezoelectric, Raman intensity spectrum, electronic structure, first-principles calculations, solid state synthesis, photocatalysis, hydrothermal synthesis

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Authors: Nadine Raidl, Benjamin Kaufmann, Michael Hofstätter, Peter Supancic

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If polycrystalline ZnO is properly doped and sintered under very specific conditions, it shows unique electrical properties, which are indispensable for today’s electronic industries, where it is used as the number one overvoltage protection material. Under a critical voltage, the polycrystalline bulk exhibits high electrical resistance but becomes suddenly up to twelve magnitudes more conductive if this voltage limit is exceeded (i.e., varistor effect). It is known that these peerless properties have their origin in the grain boundaries of the material. Electric charge is accumulated in the boundaries, causing a depletion layer in their vicinity and forming potential barriers (so-called Double Schottky Barriers, or DSB) which are responsible for the highly non-linear conductivity. Since ZnO is a piezoelectric material, mechanical stresses induce polarisation charges that modify the DSB heights and as a result the global electrical characteristics (i.e., piezotronic effect). In this work, a finite element method was used to simulate emerging stresses on individual grains in the bulk. Besides, experimental efforts were made to testify a coherent model that could explain this influence. Electron back scattering diffraction was used to identify grain orientations. With the help of wet chemical etching, grain polarization was determined. Micro lock-in infrared thermography (MLIRT) was applied to detect current paths through the material, and a micro 4-point probes method system (M4PPS) was employed to investigate current-voltage characteristics between single grains. Bulk samples were tested under uniaxial pressure. It was found that the conductivity can increase by up to three orders of magnitude with increasing stress. Through in-situ MLIRT, it could be shown that this effect is caused by the activation of additional current paths in the material. Further, compressive tests were performed on miniaturized samples with grain paths containing solely one or two grain boundaries. The tests evinced both an increase of the conductivity, as observed for the bulk, as well as a decreased conductivity. This phenomenon has been predicted theoretically and can be explained by piezotronically induced surface charges that have an impact on the DSB at the grain boundaries. Depending on grain orientation and stress direction, DSB can be raised or lowered. Also, the experiments revealed that the conductivity within one single specimen can increase and decrease, depending on the current direction. This novel finding indicates the existence of asymmetric Double Schottky Barriers, which was furthermore proved by complementary methods. MLIRT studies showed that the intensity of heat generation within individual current paths is dependent on the direction of the stimulating current. M4PPS was used to study the relationship between the I-V characteristics of single grain boundaries and grain orientation and revealed asymmetric behavior for very specific orientation configurations. A new model for the Double Schottky Barrier, taking into account the natural asymmetry and explaining the experimental results, will be given.

Keywords: Asymmetric Double Schottky Barrier, piezotronic, varistor, zinc oxide

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Authors: Hend Ben Tkhayat , Khaled Al Zahabi, Husam Younes

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Introduction: Vildagliptin (VG), a dipeptidyl peptidase-4 inhibitor (DPP-4), was proven to be an active agent for the treatment of type 2 diabetes. VG works by enhancing and prolonging the activity of incretins which improves insulin secretion and decreases glucagon release, therefore lowering blood glucose level. It is usually used with various classes, such as insulin sensitizers or metformin. VG is currently only marketed as an immediate-release tablet that is administered twice daily. In this project, we aim to formulate an extended-release with a zero-order profile tableted lipid microparticles of VG that could be administered once daily ensuring the patient’s convenience. Method: The spray-congealing technique was used to prepare VG microparticles. Compritol® was heated at 10 oC above its melting point and VG was dispersed in the molten carrier using a homogenizer (IKA T25- USA) set at 13000 rpm. VG dispersed in the molten Compritol® was added dropwise to the molten Gelucire® 50/13 and PEG® (400, 6000, and 35000) in different ratios under manual stirring. The molten mixture was homogenized and Carbomer® amount was added. The melt was pumped through the two-fluid nozzle of the Buchi® Spray-Congealer (Buchi B-290, Switzerland) using a Pump drive (Master flex, USA) connected to a silicone tubing wrapped with silicone heating tape heated at the same temperature of the pumped mix. The physicochemical properties of the produced VG-loaded microparticles were characterized using Mastersizer, Scanning Electron Microscope (SEM), Differential Scanning Calorimeter (DSC) and X‐Ray Diffractometer (XRD). VG microparticles were then pressed into tablets using a single punch tablet machine (YDP-12, Minhua pharmaceutical Co. China) and in vitro dissolution study was investigated using Agilent Dissolution Tester (Agilent, USA). The dissolution test was carried out at 37±0.5 °C for 24 hours in three different dissolution media and time phases. The quantitative analysis of VG in samples was realized using a validated High-Pressure Liquid Chromatography (HPLC-UV) method. Results: The microparticles were spherical in shape with narrow distribution and smooth surface. DSC and XRD analyses confirmed the crystallinity of VG that was lost after being incorporated into the amorphous polymers. The total yields of the different formulas were between 70% and 80%. The VG content in the microparticles was found to be between 99% and 106%. The in vitro dissolution study showed that VG was released from the tableted particles in a controlled fashion. The adjustment of the hydrophilic/hydrophobic ratio of excipients, their concentration and the molecular weight of the used carriers resulted in tablets with zero-order kinetics. The Gelucire 50/13®, a hydrophilic polymer was characterized by a time-dependent profile with an important burst effect that was decreased by adding Compritol® as a lipophilic carrier to retard the release of VG which is highly soluble in water. PEG® (400,6000 and 35 000) were used for their gelling effect that led to a constant rate delivery and achieving a zero-order profile. Conclusion: Tableted spray-congealed lipid microparticles for extended-release of VG were successfully prepared and a zero-order profile was achieved.

Keywords: vildagliptin, spray congealing, microparticles, controlled release

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Authors: Jacques M. Berner, Lehlogonolo Maloma

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Context: Glyphosate, a widely used herbicide, has raised concerns about its impact on various crops. Amaranthus cruentus, an important grain crop species, is particularly susceptible to glyphosate. Understanding the specific disruptions caused by glyphosate on the photosynthetic process in Amaranthus cruentus is crucial for assessing its effects on crop productivity and ecological sustainability. Research Aim: This study aimed to investigate the dose-dependent impact of glyphosate on the photochemical efficiency of Amaranthus cruentus using the OJIP transient analysis. The goal was to assess the specific disruptions caused by glyphosate on key parameters of photosystem II. Methodology: The experiment was conducted in a controlled greenhouse environment. Amaranthus cruentus plants were exposed to different concentrations of glyphosate, including half, recommended, and double the recommended application rates. The photochemical efficiency of the plants was evaluated using non-invasive chlorophyll a fluorescence measurements and subsequent analysis of OJIP transients. Measurements were taken on 1-hour dark-adapted leaves using a Hansatech Handy PEA+ chlorophyll fluorimeter. Findings: The study's results demonstrated a significant reduction in the photochemical efficiency of Amaranthus cruentus following glyphosate treatment. The OJIP transients showed distinct alterations in the glyphosate-treated plants compared to the control group. These changes included a decrease in maximal fluorescence (FP) and a delay in the rise of the fluorescence signal, indicating impairment in the energy conversion process within the photosystem II. Glyphosate exposure also led to a substantial decrease in the maximum quantum yield efficiency of photosystem II (FV/FM) and the total performance index (PItotal), which reflects the overall photochemical efficiency of photosystem II. These reductions in photochemical efficiency were observed even at half the recommended dose of glyphosate. Theoretical Importance: The study provides valuable insights into the specific disruptions caused by glyphosate on the photochemical efficiency of Amaranthus cruentus. Data Collection and Analysis Procedures: Data collection involved non-invasive chlorophyll a fluorescence measurements using a chlorophyll fluorimeter on dark-adapted leaves. The OJIP transients were then analyzed to assess specific disruptions in key parameters of photosystem II. Statistical analysis was conducted to determine the significance of the differences observed between glyphosate-treated plants and the control group. Question Addressed: The study aimed to address the question of how glyphosate exposure affects the photochemical efficiency of Amaranthus cruentus, specifically examining disruptions in the photosynthetic electron transport chain and overall photochemical efficiency. Conclusion: The study demonstrates that glyphosate severely impairs the photochemical efficiency of Amaranthus cruentus, as indicated by the alterations in OJIP transients. Even at half the recommended dose, glyphosate caused significant reductions in photochemical efficiency. These findings highlight the detrimental effects of glyphosate on crop productivity and emphasize the need for further research to evaluate its long-term consequences and ecological implications in agriculture. The authors gratefully acknowledge the support from North-West University for making this research possible.

Keywords: glyphosate, amaranthus cruentus, ojip transient analysis, pitotal, photochemical efficiency, chlorophyll fluorescence, weeds

Procedia PDF Downloads 91

Authors: S. Mamoucha, N.Tsafantakis, T. Ioannidis, S. Chatzipanagiotou, C. Nikolaou, L. Skaltsounis, N. Fokialakis, N. Christodoulakis

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Introduction: Pistacia lentiscus L. (well known as Mastic tree) is an evergreen sclerophyllous shrub that extensively thrives in the eastern Mediterranean area yet only the trees cultivated in the southern region of the Greek island Chios produces mastic resin. Different parts of P. lentiscus L. var. chia have been used in folk medicine for various purposes, such as tonic, aphrodisiac, antiseptic, antihypertensive and management of dental, gastrointestinal, liver, urinary, and respiratory tract disorders. Several studies have focused on the antibacterial activity of its resin (gum) and its essential oil. However, there is no study combining anatomy of the plant organs, phytochemical profile, and antibacterial screening of the plant. In our attempt to discover novel bioactive metabolites from the mastic tree, we screened its antibacterial activity not only against ATCC strains but also against clinical, resistant strains. Materials-methods: Leaves were investigated using Transmission (ΤΕΜ) and Scanning Εlectron Microscopy (SEM). Histochemical tests were performed on fresh and fixed tissue. Extracts prepared from dried, powdered leaves using 3 different solvents (DCM, MeOH and H2O) the waste water obtained after a hydrodistillation process for essential oil production were screened for their phytochemical content and antibacterial activity. Μetabolite profiling of polar and non-polar extracts was recorded by GC-MS and LC-HRMS techniques and analyzed using in-house and commercial libraries. The antibacterial screening was performed against Staphylococcus aureus ATCC25923, Escherichia coli ATCC25922, Pseudomonas aeruginosa ATCC27853 and against clinical, resistant strains Methicillin-resistant S. aureus (MRSA), Carbapenem-Resistant Metallo-β-Lactamase (carbapenemase) P. aeruginosa (VIM), Klebsiella pneumoniae carbapenemases (KPCs) and Acinetobacter baumanii resistant strains. The antibacterial activity was tested by the Kirby Bauer and the Agar Well Diffusion method. The zone of inhibition (ZI) of each extract was measured and compared with those of common antibiotics. Results: Leaf is compact with inosclereids and numerous idioblasts containing a globular, spiny crystal. The major nerves of the leaf contain a resin duct. Mesophyll cells showed accumulation of osmiophillic metabolites. Histochemical treatments defined secondary metabolites in subcellular localization. The phytochemical investigation revealed the presence of a large number of secondary metabolites, belonging to different chemical groups, such as terpenoids, phenolic compounds (mainly myricetin, kaempferol and quercetin glycosides), phenolic, and fatty acids. Among the extracts, the hydrostillation wastewater achieved the best results against most of the bacteria tested. MRSA, VIM and A. baumanii were inhibited. Conclusion: Extracts from plants have recently been of great interest with respect to their antimicrobial activity. Their use emerged from a growing tendency to replace synthetic antimicrobial agents with natural ones. Leaves of P. lentiscus L. var. chia showed a high antimicrobial activity even against drug - resistant bacteria. Future prospects concern the better understanding of mode of action of the antibacterial activity, the isolation of the most bioactive constituents and the clarification if the activity is related to a single compound or to the synergistic effect of several ones.

Keywords: antibacterial screening, leaf anatomy, phytochemical profile, Pistacia lentiscus var. chia

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Authors: E. Mosiniewicz-Szablewska, P. Suchocki, P. C. Morais

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Despite the significant progress in cancer treatment, there is a need to search for new therapeutic methods in order to minimize side effects. Chemotherapy, the main current method of treating cancer, is non-selective and has a number of limitations. Toxicity to healthy cells is undoubtedly the biggest problem limiting the use of many anticancer drugs. The problem of how to kill cancer without harming a patient can be solved by using organic selenium (IV) compounds. Organic selenium (IV) compounds are a new class of materials showing a strong anticancer activity. They are first organic compounds containing selenium at the +4 oxidation level and therefore they eliminate the multidrug-resistance for all tumor cell lines tested so far. These materials are capable of selectively killing cancer cells without damaging the healthy ones. They are obtained by the incorporation of selenous acid (H2SeO3) into molecules of fatty acids of sunflower oil and therefore, they are inexpensive to manufacture. Attaching these compounds to magnetic carriers enables their precise delivery directly to the tumor area and the simultaneous application of the magnetic hyperthermia, thus creating a huge opportunity to effectively get rid of the tumor without any side effects. Polylactic-co-glicolic acid (PLGA) nanocapsules loaded with maghemite (-Fe2O3) nanoparticles and organic selenium (IV) compounds are successfully prepared by nanoprecipitation method. In vitro antitumor activity of the nanocapsules were evidenced using murine melanoma (B16-F10), oral squamos carcinoma (OSCC) and murine (4T1) and human (MCF-7) breast lines. Further exposure of these cells to an alternating magnetic field increased the antitumor effect of nanocapsules. Moreover, the nanocapsules presented antitumor effect while not affecting normal cells. Magnetic properties of the nanocapsules were investigated by means of dc magnetization, ac susceptibility and electron spin resonance (ESR) measurements. The nanocapsules presented a typical superparamagnetic behavior around room temperature manifested itself by the split between zero field-cooled/field-cooled (ZFC/FC) magnetization curves and the absence of hysteresis on the field-dependent magnetization curve above the blocking temperature. Moreover, the blocking temperature decreased with increasing applied magnetic field. The superparamagnetic character of the nanocapsules was also confirmed by the occurrence of a maximum in temperature dependences of both real ′(T) and imaginary ′′ (T) components of the ac magnetic susceptibility, which shifted towards higher temperatures with increasing frequency. Additionally, upon decreasing the temperature the ESR signal shifted to lower fields and gradually broadened following closely the predictions for the ESR of superparamagnetoc nanoparticles. The observed superparamagnetic properties of nanocapsules enable their simple manipulation by means of magnetic field gradient, after introduction into the blood stream, which is a necessary condition for their use as magnetic drug carriers. The observed anticancer and superparamgnetic properties show that the magnetic nanocapsules loaded with organic selenium (IV) compounds should be considered as an effective material system for magnetic drug delivery and magnetohyperthermia inductor in antitumor therapy.

Keywords: cancer treatment, magnetic drug delivery system, nanomaterials, nanotechnology

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Authors: T. Ul Rehman, S. Agnello, F. M. Gelardi, M. M. Calvino, G. Lazzara, G. Buscarino, M. Cannas

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Metal-Organic Frameworks (MOFs) have emerged as promising candidates for detecting metal ions owing to their large surface area, customizable porosity, and diverse functionalities. In recent years, there has been a surge in research focused on MOFs with luminescent properties. These frameworks are constructed through coordinated bonding between metal ions and multi-dentate ligands, resulting in inherent fluorescent structures. Their luminescent behavior is influenced by factors like structural composition, surface morphology, pore volume, and interactions with target analytes, particularly metal ions. MOFs exhibit various sensing mechanisms, including photo-induced electron transfer (PET) and charge transfer processes such as ligand-to-metal (LMCT) and metal-to-ligand (MLCT) transitions. Among these, MIL-53(Al) stands out due to its flexibility, stability, and specific affinity towards certain metal ions, making it a promising platform for selective metal ion sensing. This study investigates the structural, thermal, and luminescent properties of MIL-53(Al) metal-organic framework (MOF) upon Fe3+ cation exchange. Two separate sets of samples were prepared to activate the MOF powder at different temperatures. The first set of samples, referred to as MIL-53(Al), activated (120°C), was prepared by activating the raw powder in a glass tube at 120°C for 12 hours and then sealing it. The second set of samples, referred to as MIL-53(Al), activated (300°C), was prepared by activating the MIL-53(Al) powder in a glass tube at 300°C for 70 hours. Additionally, 25 mg of MIL-53(Al) powder was dispersed in 5 mL of Fe3+ solution at various concentrations (0.1-100 mM) for the cation exchange experiment. The suspension was centrifuged for five minutes at 10,000 rpm to extract MIL-53(Al) powder. After three rounds of washing with ultrapure water, MIL-53(Al) powder was heated at 120°C for 12 hours. For PXRD and TGA analyses, a sample of the obtained MIL-53(Al) was used. We also activated the cation-exchanged samples for time-resolved photoluminescence (TRPL) measurements at two distinct temperatures (120 and 300°C) for comparative analysis. Powder X-ray diffraction patterns reveal amorphization in samples with higher Fe3+ concentrations, attributed to alterations in coordination environments and ion exchange dynamics. Thermal decomposition analysis shows reduced weight loss in Fe3+-exchanged MOFs, indicating enhanced stability due to stronger metal-ligand bonds and altered decomposition pathways. Raman spectroscopy demonstrates intensity decrease, shape disruption, and frequency shifts, indicative of structural perturbations induced by cation exchange. Photoluminescence spectra exhibit ligand-based emission (π-π* or n-π*) and ligand-to-metal charge transfer (LMCT), influenced by activation temperature and Fe3+ incorporation. Quenching of luminescence intensity and shorter lifetimes upon Fe3+ exchange result from structural distortions and Fe3+ binding to organic linkers. In a nutshell, this research underscores the complex interplay between composition, structure, and properties in MOFs, offering insights into their potential for diverse applications in catalysis, gas storage, and luminescent devices.

Keywords: Fe³⁺ cation exchange, luminescent metal-organic frameworks (LMOFs), MIL-53(Al), solid-state analysis

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Authors: Dmitriy Berillo, Areej K. A. Al-Jwaid, Jonathan L. Caplin, Andrew Cundy, Irina Savina

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Chlorophenols (CPs) are used as a precursor in the production of higher CPs and dyestuffs, and as a preservative. Contamination by CPs of the ground water is located in the range from 0.15-100mg/L. The EU has set maximum concentration limits for pesticides and their degradation products of 0.1μg/L and 0.5μg/L, respectively. People working in industries which produce textiles, leather products, domestic preservatives, and petrochemicals are most heavily exposed to CPs. The International Agency for Research on Cancers categorized CPs as potential human carcinogens. Existing multistep water purification processes for CPs such as hydrogenation, ion exchange, liquid-liquid extraction, adsorption by activated carbon, forward and inverse osmosis, electrolysis, sonochemistry, UV irradiation, and chemical oxidation are not always cost effective and can cause the formation of even more toxic or mutagenic derivatives. Bioremediation of CPs derivatives utilizing microorganisms results in 60 to 100% decontamination efficiency and the process is more environmentally-friendly compared with existing physico-chemical methods. Microorganisms immobilized onto a substrate show many advantages over free bacteria systems, such as higher biomass density, higher metabolic activity, and resistance to toxic chemicals. They also enable continuous operation, avoiding the requirement for biomass-liquid separation. The immobilized bacteria can be reused several times, which opens the opportunity for developing cost-effective processes for wastewater treatment. In this study, we develop a bioremediation system for CPs based on macroporous materials, which can be efficiently used for wastewater treatment. Conditions for the preparation of the macroporous material from specific bacterial strains (Pseudomonas mendocina and Rhodococus koreensis) were optimized. The concentration of bacterial cells was kept constant; the difference was only the type of cross-linking agents used e.g. glutaraldehyde, novel polymers, which were utilized at concentrations of 0.5 to 1.5%. SEM images and rheology analysis of the material indicated a monolithic macroporous structure. Phenol was chosen as a model system to optimize the function of the cryogel material and to estimate its enzymatic activity, since it is relatively less toxic and harmful compared to CPs. Several types of macroporous systems comprising live bacteria were prepared. The viability of the cross-linked bacteria was checked using Live/Dead BacLight kit and Laser Scanning Confocal Microscopy, which revealed the presence of viable bacteria with the novel cross-linkers, whereas the control material cross-linked with glutaraldehyde(GA), contained mostly dead cells. The bioreactors based on bacteria were used for phenol degradation in batch mode at an initial concentration of 50mg/L, pH 7.5 and a temperature of 30°C. Bacterial strains cross-linked with GA showed insignificant ability to degrade phenol and for one week only, but a combination of cross-linking agents illustrated higher stability, viability and the possibility to be reused for at least five weeks. Furthermore, conditions for CPs degradation will be optimized, and the chlorophenol degradation rates will be compared to those for phenol. This is a cutting-edge bioremediation approach, which allows the purification of waste water from sustainable compounds without a separation step to remove free planktonic bacteria. Acknowledgments: Dr. Berillo D. A. is very grateful to Individual Fellowship Marie Curie Program for funding of the research.

Keywords: bioremediation, cross-linking agents, cross-linked microbial cell, chlorophenol degradation

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Authors: Chunyang Miao, Bingxin Li, Shanglong Ning, Christopher J. B. Ford

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While it is challenging to fabricate electronic devices close to atomic dimensions in conventional top-down lithography, molecular electronics is promising to help maintain the exponential increase in component densities via using molecular building blocks to fabricate electronic components from the bottom up. It offers smaller, faster, and more energy-efficient electronic and photonic systems. A self-assembled monolayer (SAM) of molecules is a layer of molecules that self-assembles on a substrate. They are mechanically flexible, optically transparent, low-cost, and easy to fabricate. A large-area multi-layer structure has been designed and investigated by the team, where a SAM of designed molecules is sandwiched between graphene and gold electrodes. Each molecule can act as a quantum dot, with all molecules conducting in parallel. When a source-drain bias is applied, significant current flows only if a molecular orbital (HOMO or LUMO) lies within the source-drain energy window. If electrons tunnel sequentially on and off the molecule, the charge on the molecule is well-defined and the finite charging energy causes Coulomb blockade of transport until the molecular orbital comes within the energy window. This produces ‘Coulomb diamonds’ in the conductance vs source-drain and gate voltages. For different tunnel barriers at either end of the molecule, it is harder for electrons to tunnel out of the dot than in (or vice versa), resulting in the accumulation of two or more charges and a ‘Coulomb staircase’ in the current vs voltage. This nanostructure exhibits highly reproducible Coulomb-staircase patterns, together with additional oscillations, which are believed to be attributed to molecular vibrations. Molecules are more isolated than semiconductor dots, and so have a discrete phonon spectrum. When tunnelling into or out of a molecule, one or more vibronic states can be excited in the molecule, providing additional transport channels and resulting in additional peaks in the conductance. For useful molecular electronic devices, achieving the optimum orbital alignment of molecules to the Fermi energy in the leads is essential. To explore it, a drop of ionic liquid is employed on top of the graphene to establish an electric field at the graphene, which screens poorly, gating the molecules underneath. Results for various molecules with different alignments of Fermi energy to HOMO have shown highly reproducible Coulomb-diamond patterns, which agree reasonably with DFT calculations. In summary, this large-area SAM molecular junction is a promising candidate for future electronic circuits. (1) The small size (1-10nm) of the molecules and good flexibility of the SAM lead to the scalable assembly of ultra-high densities of functional molecules, with advantages in cost, efficiency, and power dissipation. (2) The contacting technique using graphene enables mass fabrication. (3) Its well-observed Coulomb blockade behaviour, narrow molecular resonances, and well-resolved vibronic states offer good tuneability for various functionalities, such as switches, thermoelectric generators, and memristors, etc.

Keywords: molecular electronics, Coulomb blokade, electron-phonon coupling, self-assembled monolayer

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Authors: Huan Peng, Chenye Zeng, Zhao Wang

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Alzheimer’s disease (AD) is an age-related neurodegenerative disease that is a leading cause of dementia syndromes and has become a huge burden on society and families. The main pathological features of AD involve excessive deposition of β-amyloid (Aβ) and Tau proteins in the brain, resulting in loss of neurons, expansion of neuroinflammation, and cognitive dysfunction in patients. Researchers have found effective drugs to clear the brain of error-accumulating proteins or to slow the loss of neurons, but their direct administration has key bottlenecks such as single-drug limitation, rapid blood clearance rate, impenetrable blood-brain barrier (BBB), and poor ability to target tissues and cells. Therefore, we are committed to seeking a suitable and efficient delivery system. Inspired by the possibility that exosomes may be involved in the secretion and transport mechanism of many signaling molecules or proteins in the brain, exosomes have attracted extensive attention as natural nanoscale drug carriers. We selected exosomes derived from bone marrow mesenchymal stem cells (MSC-EXO) with low immunogenicity and exosomes derived from hippocampal neurons (HT22-EXO) that may have excellent homing ability to overcome the deficiencies of oral or injectable pathways and bypass the BBB through nasal administration and evaluated their delivery ability and effect on AD. First, MSC-EXO and HT22 cells were isolated and cultured, and MSCs were identified by microimaging and flow cytometry. Then MSC-EXO and HT22-EXO were obtained by gradient centrifugation and qEV SEC separation column, and a series of physicochemical characterization were performed by transmission electron microscope, western blot, nanoparticle tracking analysis and dynamic light scattering. Next, exosomes labeled with lipophilic fluorescent dye were administered to WT mice and APP/PS1 mice to obtain fluorescence images of various organs at different times. Finally, APP/PS1 mice were administered intranasally with two exosomes 20 times over 40 days and 20 μL each time. Behavioral analysis and pathological section analysis of the hippocampus were performed after the experiment. The results showed that MSC-EXO and HT22-EXO were successfully isolated and characterized, and they had good biocompatibility. MSC-EXO showed excellent brain enrichment in APP/PS1 mice after intranasal administration, could improve the neuronal damage and reduce inflammation levels in the hippocampus of APP/PS1 mice, and the improvement effect was significantly better than HT22-EXO. However, intranasal administration of the two exosomes did not cause depression and anxious-like phenotypes in APP/PS1 mice, nor significantly improved the short-term or spatial learning and memory ability of APP/PS1 mice, and had no significant effect on the content of Aβ plaques in the hippocampus, which also meant that MSC-EXO could use their own advantages in combination with other drugs to clear Aβ plaques. The possibility of realizing highly effective non-invasive synergistic treatment for AD provides new strategies and ideas for clinical research.

Keywords: Alzheimer’s disease, exosomes derived from mesenchymal stem cell, intranasal administration, therapy-carrier dual roles

Procedia PDF Downloads 62

Authors: Seema Kothari, Dinesh Panday

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An observed correlation of the reaction rates with the changes in the nature of substituent present on one of the reactants often reveals the nature of transition state. Selective oxidation of organic compounds under non-aqueous media is an important transformation in synthetic organic chemistry. Inorganic chromates and dichromates being drastic oxidant and are generally insoluble in most organic solvents, a number of different chromium (VI) derivatives have been synthesized. Benzimidazolium dichromate (BIDC) is one of the recently reported Cr(VI) reagents which is neither hygroscopic nor light sensitive being, therefore, much stable. Not many reports on the kinetics of the oxidations by BIDC are seemed to be available in the literature. In the present investigation, the kinetics and mechanism of benzyl alcohol (BA) and a number of para- and meta-substituted benzyl alcohols by benzimidazolium dichromate (BIDC), in dimethyl sulphoxide, is reported. The reactions were followed spectrophotometrically at 364 nm by monitoring the decrease in [BIDC] for up to 85-90% reaction, the temperature being constant. The observed oxidation product is the corresponding benzaldehyde. The reactions were of first order with respect to each the alcohol and BIDC. The reactions are catalyzed by proton, and the dependence is of the form: kobs = a + b[H+]. The reactions thus follow both, an acid-dependent and acid-independent paths. The oxidation of [1,1 2H2]benzyl alcohol exhibited the presence of a substantial kinetic isotope effect ( kH/kD = 6.20 at 298 K ). This indicated the cleavage of a α-C-H bond in the rate-determining step. An analysis of the temperature dependence of the deuterium isotope effect showed that the loss of hydrogen proceeds through a concerted cyclic process. The rate of oxidation of BA was determined in 19 organic solvents. An analysis of the solvent effect by Swain’s equation indicated that though both the anion and cation-solvating powers of the solvent contribute to the observed solvent effect, the role of cation-solvation is major. The rates of the para and meta compounds, at 298 K, failed to exhibit a significant correlation in terms of Hammett or Brown's substituent constants. The rates were then subjected to analyses in terms of dual substituent parameter (DSP) equations. The rates of oxidation of the para-substituted benzyl alcohols show an excellent correlation with Taft's σI and σRBA values. However, the rates for the meta-substituted benzyl alcohols show an excellent correlation with σI and σR0. The polar reaction constants are negative indicating an electron-deficient transition state. Hence the overall mechanism is proposed to involve the formation of a chromate ester in a fast pre-equilibrium and then a decomposition of the ester in a subsequent slow step via a cyclic concerted symmetrical transition state, involving hydride-ion transfer, leading to the product. The first order dependence on alcohol may be accounted in terms of the small value of the formation constant of the ester intermediate. An another reaction mechanism accounting the acid-catalysis involve the formation of a protonated BIDC prior to formation of an ester intermediate which subsequently decomposes in a slow step leading to the product.

Keywords: benzimidazolium dichromate, benzyl alcohols, correlation analysis, kinetics, oxidation

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Authors: Ibrahim Abdulla Labib, Medhat Mohamed Morsy, Gamal Hosny, Hanan Dawood Yassa, Gaber Hassan

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Amiodarone is a very effective drug, widely used for arrhythmia. Unfortunately it has many side effects involving many organs especially thyroid gland. The current work was conducted to elucidate the effect of amiodarone on the thyroid gland and the possible protective role of vitamin E. Fifty adult male albino rats weighed 200 – 250 grams were divided into five groups; ten rats each. Group I (Control): Five rats were sacrificed after three weeks and five rats were sacrificed after six weeks. Group II (Sham control): Each rat received sunflower oil orally; the solvent of vitamin E for three weeks. Group III (Amiodarone-treated): each rat received an oral dose of amiodarone; 150 mg/kg/day for three weeks. Group IV (Recovery): Each rat received amiodarone as group III then the drug was stopped for three weeks to evaluate recovery. Group V (Amiodarone + Vitamin E-treated): Each rat received amiodarone as group III followed by 100 mg/kg/day vitamin E orally for three weeks. Thyroid gland of the sacrificed animals were dissected out and prepared for light and electron microscopic studies. Amiodarone administration resulted in loss of normal follicular architecture as many follicles appeared either shrunken, empty or contained scanty pale colloid. Some follicles appeared lined by more than one layer of cells while others showed interruption of their membrane. Masson's Trichrome stained sections showed increased collagen fibers in between the thyroid follicles. Ultrastructurally, the apical border of the follicular cells showed few irregular detached microvilli. The nuclei of the follicular cells were almost irregular with chromatin condensation. The cytoplasm of most follicular cells revealed numerous dilated rough endoplasmic reticulum with numerous lysosomes. After three weeks of stopping amiodarone, the follicles were nearly regular in outline. Some follicles were filled with homogenous eosinophilic colloid and others had shrunken pale colloid or were empty. Some few follicles showed exfoliated cells in their lumina and others were still lined by more than one layer of follicular cells. Moderate amounts of collagen fibers were observed in-between thyroid follicles. Ultrastructurally, many follicular cells had rounded euchromatic nucleui, moderate number of lysosomes and moderately dilated rough endoplasmic reticulum. However, few follicular cells still showing irregular nucleui, dilated rough endoplasmic reticulum and many cytoplasmic vacuoles. Administration of vitamin E with amiodarone for three weeks resulted in obvious structural improvement. Most of the follicles were lined by a single layer of cuboidal cells and the lumina were filled with homogenous eosinophilic colloid with very few vacuolations. The majority of follicular cells had rounded nuclei with occasional detection of ballooned cells and dark nuclei. Scanty collagen fibers were detected among thyroid follicles. Ultrastructurally, most follicular cells exhibited rounded euchromatic nuclei with few short microvilli were projecting into the colloid. Few lysosomes were also noticed. It was concluded that amiodarone administration leads to many adverse histological changes in the thyroid gland. Some of these changes are reversible during the recovery period however concomitant vitamin E administration with amiodarone has a major protective role in preventing many of these changes.

Keywords: amiodarone, recovery, ultrastructure, vitamin E.

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Authors: Glauco M. M. M. Lustosa, João Paulo C. Costa, Leinig Antônio Perazolli, Maria Aparecida Zaghete

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SnO2 has electrical conductivity due to the excess of electrons and structural defects, being its electrical behavior highly dependent on sintering temperature and chemical composition. The addition of metals modifiers into the crystalline structure can improve and controlling the behavior of some semiconductor oxides that can therefore develop different applications such as varistors (ceramic with non-ohmic behavior between current and voltage, i.e. conductive during normal operation and resistive during overvoltage). The polymeric precursor method, based on the complexation reaction between metal ion and policarboxylic acid and then polymerized with ethylene glycol, was used to obtain nanopowders ceramic. The metal immobilization reduces its segregation during the decomposition of the polyester resulting in a crystalline oxide with high chemical homogeneity. The preparation of films from ceramics nanoparticles using electrophoretic deposition method (EPD) brings prospects for a new generation of smaller size devices with easy integration technology. EPD allows to control time and current and therefore it can have control of the thickness, surface roughness and the film density, quickly and with low production costs. The sintering process is key to control size and grain boundary density of the film. In this step, there is the diffusion of metals that promote densification and control of intrinsic defects or change these defects which will form and modify the potential barrier in the grain boundary. The use of microwave oven for sintering is an advantageous process due to the fast and homogeneous heating rate, promoting the diffusion and densification without irregular grain growth. This research was done a comparative study of sintering temperature by use of zinc as modifier agent to verify the influence on sintering step aiming to promote densification and grain growth, which influences the potential barrier formation and then changed the electrical behavior. SnO2-nanoparticles were obtained with 1 %mol of ZnO + 0.05 %mol of Nb2O5 (SZN), deposited as film through EPD (voltage 2 kV, time of 10 min) on Si/Pt substrate. Sintering was made in a microwave oven at 800, 900 and 1000 °C. For complete coverage of the substrate by nanoparticles with low surface roughness and uniform thickness was added 0.02 g of solid iodine in alcoholic suspension SnO2 to increase particle surface charge. They were also used magneto in EPD system that improved the deposition rate forming a compact film. Using a scanning electron microscope of high resolution (SEM_FEG) it was observed nanoparticles with average size between 10-20 nm, after sintering the average size was 150 to 200 nm and thickness of 5 µm. Also, it was verified that the temperature at 1000 °C was the most efficient in sintering. The best sintering time was also recorded and determined as 40 minutes. After sintering, the films were recovered with Cr3+ ions layer by EPD, then the films were again thermally treated. The electrical characterizations (nonlinear coefficient of 11.4, voltage rupture of ~60 V and leakage current = 4.8x10−6 A), allow considering the new methodology suitable for prepare SnO2-based varistor applied for development of electrical protection devices for low voltage.

Keywords: chemical synthesis, electrophoretic deposition, microwave sintering, tin dioxide

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Authors: Rubens P. Costa, Marcelo A. Leigui de Oliveira

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The comprehension of features on the energy spectra, the chemical compositions, and the origins of Ultra-High Energy Cosmic Rays (UHECRs) - mainly atomic nuclei with energies above ~1.0 EeV (exa-electron volts) - are intrinsically linked to the problem of determining the magnitude of their deflections in cosmic magnetic fields on cosmological scales. In addition, as they propagate from the source to the observer, modifications are expected in their original energy spectra, anisotropy, and the chemical compositions due to interactions with low energy photons and matter. This means that any consistent interpretation of the nature and origin of UHECRs has to include the detailed knowledge of their propagation in a three-dimensional environment, taking into account the magnetic deflections and energy losses. The parameter space range for the magnetic fields in the universe is very large because the field strength and especially their orientation have big uncertainties. Particularly, the strength and morphology of the Extragalactic Magnetic Fields (EGMFs) remain largely unknown, because of the intrinsic difficulty of observing them. Monte Carlo simulations of charged particles traveling through a simulated magnetized universe is the straightforward way to study the influence of extragalactic magnetic fields on UHECRs propagation. However, this brings two major difficulties: an accurate numerical modeling of charged particles diffusion in magnetic fields, and an accurate numerical modeling of the magnetized Universe. Since magnetic fields do not cause energy losses, it is important to impose that the particle tracking method conserve the particle’s total energy and that the energy changes are results of the interactions with background photons only. Hence, special attention should be paid to computational effects. Additionally, because of the number of particles necessary to obtain a relevant statistical sample, the particle tracking method must be computationally efficient. In this work, we present an analysis of the propagation of ultra-high energy charged particles in the intergalactic medium. The EGMFs are considered to be coherent within cells of 1 Mpc (mega parsec) diameter, wherein they have uniform intensities of 1 nG (nano Gauss). Moreover, each cell has its field orientation randomly chosen, and a border region is defined such that at distances beyond 95% of the cell radius from the cell center smooth transitions have been applied in order to avoid discontinuities. The smooth transitions are simulated by weighting the magnetic field orientation by the particle's distance to the two nearby cells. The energy losses have been treated in the continuous approximation parameterizing the mean energy loss per unit path length by the energy loss length. We have shown, for a particle with the typical energy of interest the integration method performance in the relative error of Larmor radius, without energy losses and the relative error of energy. Additionally, we plotted the distance amplification from rectilinear propagation as a function of the traveled distance, particle's magnetic rigidity, without energy losses, and particle's energy, with energy losses, to study the influence of particle's species on these calculations. The results clearly show when it is necessary to use a full three-dimensional simulation.

Keywords: cosmic rays propagation, extragalactic magnetic fields, magnetic deflections, ultra-high energy

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Authors: Mohamed Sifan, Brabha Nagaratnam, Julian Thamboo, Keerthan Poologanathan

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Ultra high performance concrete (UHPC) is a type of cementitious material known for its exceptional strength, ductility, and durability. However, its production is often associated with high costs due to the significant amount of cementitious materials required and the use of fine powders to achieve the desired strength. The aim of this research is to explore the feasibility of developing cost-effective UHPC mixes using locally available materials. Specifically, the study aims to investigate the use of coarse limestone sand along with other sand types, namely, basalt sand, dolomite sand, and river sand for developing UHPC mixes and evaluating its performances. The study utilises the particle packing model to develop various UHPC mixes. The particle packing model involves optimising the combination of coarse limestone sand, basalt sand, dolomite sand, and river sand to achieve the desired properties of UHPC. The developed UHPC mixes are then evaluated based on their workability (measured through slump flow and mini slump value), compressive strength (at 7, 28, and 90 days), splitting tensile strength, and microstructural characteristics analysed through scanning electron microscope (SEM) analysis. The results of this study demonstrate that cost-effective UHPC mixes can be developed using locally available materials without the need for silica fume or fly ash. The UHPC mixes achieved impressive compressive strengths of up to 149 MPa at 28 days with a cement content of approximately 750 kg/m³. The mixes also exhibited varying levels of workability, with slump flow values ranging from 550 to 850 mm. Additionally, the inclusion of coarse limestone sand in the mixes effectively reduced the demand for superplasticizer and served as a filler material. By exploring the use of coarse limestone sand and other sand types, this study provides valuable insights into optimising the particle packing model for UHPC production. The findings highlight the potential to reduce costs associated with UHPC production without compromising its strength and durability. The study collected data on the workability, compressive strength, splitting tensile strength, and microstructural characteristics of the developed UHPC mixes. Workability was measured using slump flow and mini slump tests, while compressive strength and splitting tensile strength were assessed at different curing periods. Microstructural characteristics were analysed through SEM and energy dispersive X-ray spectroscopy (EDS) analysis. The collected data were then analysed and interpreted to evaluate the performance and properties of the UHPC mixes. The research successfully demonstrates the feasibility of developing cost-effective UHPC mixes using locally available materials. The inclusion of coarse limestone sand, in combination with other sand types, shows promising results in achieving high compressive strengths and satisfactory workability. The findings suggest that the use of the particle packing model can optimise the combination of materials and reduce the reliance on expensive additives such as silica fume and fly ash. This research provides valuable insights for researchers and construction practitioners aiming to develop cost-effective UHPC mixes using readily available materials and an optimised particle packing approach.

Keywords: cost-effective, limestone powder, particle packing model, ultra high performance concrete

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Authors: Giulia Fredi, Andrea Dorigato, Luca Fambri, Alessandro Pegoretti

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Thermal energy storage (TES) is the storage of heat for later use, thus filling the gap between energy request and supply. The most widely used materials for TES are the organic solid-liquid phase change materials (PCMs), such as paraffin. These materials store/release a high amount of latent heat thanks to their high specific melting enthalpy, operate in a narrow temperature range and have a tunable working temperature. However, they suffer from a low thermal conductivity and need to be confined to prevent leakage. These two issues can be tackled by confining PCMs with carbon nanotubes (CNTs). TES applications include the buildings industry, solar thermal energy collection and thermal management of electronics. In most cases, TES systems are an additional component to be added to the main structure, but if weight and volume savings are key issues, it would be advantageous to embed the TES functionality directly in the structure. Such multifunctional materials could be employed in the automotive industry, where the diffusion of lightweight structures could complicate the thermal management of the cockpit environment or of other temperature sensitive components. This work aims to produce epoxy/carbon structural laminates containing CNT-stabilized paraffin. CNTs were added to molten paraffin in a fraction of 10 wt%, as this was the minimum amount at which no leakage was detected above the melting temperature (45°C). The paraffin/CNT blend was cryogenically milled to obtain particles with an average size of 50 µm. They were added in various percentages (20, 30 and 40 wt%) to an epoxy/hardener formulation, which was used as a matrix to produce laminates through a wet layup technique, by stacking five plies of a plain carbon fiber fabric. The samples were characterized microstructurally, thermally and mechanically. Differential scanning calorimetry (DSC) tests showed that the paraffin kept its ability to melt and crystallize also in the laminates, and the melting enthalpy was almost proportional to the paraffin weight fraction. These thermal properties were retained after fifty heating/cooling cycles. Laser flash analysis showed that the thermal conductivity through the thickness increased with an increase of the PCM, due to the presence of CNTs. The ability of the developed laminates to contribute to the thermal management was also assessed by monitoring their cooling rates through a thermal camera. Three-point bending tests showed that the flexural modulus was only slightly impaired by the presence of the paraffin/CNT particles, while a more sensible decrease of the stress and strain at break and the interlaminar shear strength was detected. Optical and scanning electron microscope images revealed that these could be attributed to the preferential location of the PCM in the interlaminar region. These results demonstrated the feasibility of multifunctional structural TES composites and highlighted that the PCM size and distribution affect the mechanical properties. In this perspective, this group is working on the encapsulation of paraffin in a sol-gel derived organosilica shell. Submicron spheres have been produced, and the current activity focuses on the optimization of the synthesis parameters to increase the emulsion efficiency.

Keywords: carbon fibers, carbon nanotubes, lightweight materials, multifunctional composites, thermal energy storage

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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: Sara Scolari, Davide Mombelli, Gianluca Dall'Osto, Jasna Kastivnik, Gašper Tavčar, Carlo Mapelli

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The EIT Raw Materials RIS-DustRec-II project aims to transform Electric Arc Furnace Dust (EAFD) into a valuable resource by overcoming the challenges associated with traditional recycling approaches. EAFD, a zinc-rich industrial by-product typically recycled by the Waelz process, contains complex oxides such as franklinite (ZnFe₂O₄), which hinder the efficient extraction of zinc, by also introducing other valuable elements (Fe, Ni, Cr, Cu, …) in the slag. The project aims to develop a multistage multidisciplinary approach to separate EAFD into two streams: a magnetic and non-magnetic one. In this paper the production of self-reducing briquettes from the magnetic stream of EAFD with a reducing agent, aiming to drive carbothermic reduction and recover iron as a usable alloy, was investigated. Research was focused on optimizing the magnetic and subsequent gravimetric separation (MGS) processes, followed by high-temperature smelting to evaluate reduction efficiency and phase separation. The characterization of selected two different raw EAFD samples and their magnetic-gravitational separation to isolate zinc- and iron-rich fractions was performed by X-ray diffraction and scanning electron microscope. The iron-enriched concentrates were then agglomerated into self-reducing briquettes by mixing them with either biochar (olive pomace pyrolyzed at 350 and 750°C and wood chips pyrolyzed at 750 °C) and a Cupola Furnace dust as reducing agents, combined with gelatinized corn starch as a binder. Cylindrical briquettes were produced and cured for 14 days to ensure structural integrity during subsequent thermal treatments. Smelting tests were carried out at 1400 °C in an inert argon atmosphere to assess the metallization efficiency and the separation between metal and slag phases. A carbon/oxides mass ratio of 0.262 (C/(ZnO+Fe₂O₃)) was used in these tests to maintain continuity with previous studies and to standardize reduction conditions. The magnetic and gravimetric separations effectively isolated zinc- and iron-enriched fractions, particularly for one of the two EAFD, where the concentration of Zn in the concentration fraction was reduced by 8 wt.% while Fe reached 45 wt.%. The reduction tests conducted at 1400 °C showed that the chosen carbon/oxides ratio was sufficient for the smelting of the reducible oxides within the briquettes. However, an important limitation became apparent: the amount of carbon, exceeding the stochiometric value, proved to be excessive for the effective coalescence of metal droplets, preventing clear metal-slag separation. To address this, further smelting tests were carried out in an air atmosphere rather than inert conditions to burn off excess carbon. This paper demonstrates the potential of controlled carbothermic reduction for EAFD recycling. By carefully optimizing the C/(ZnO+Fe₂O₃) ratio, the process can maximize metal recovery while achieving better separation of the metal and slag phases. This approach offers a promising alternative to traditional EAFD recycling methods, with further studies recommended to refine the parameters for industrial application.

Keywords: biochars, electrical arc furnace dust, metallization, smelting

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