Search results for: melting/solidification

Authors: Olubukayo-Opeyemi Oyetayo, Oscar Mendez-Lucio, Andreas Bender, Hans Kiefer

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The thermal melting curve of a protein provides information on its conformational stability and could provide cues on its aggregation behavior. Naturally-occurring osmolytes have been shown to improve the thermal stability of most proteins in a concentration-dependent manner. They are therefore commonly employed as additives in therapeutic protein purification and formulation. A number of intertwined and seemingly conflicting mechanisms have been put forward to explain the observed stabilizing effects, the most prominent being the preferential exclusion mechanism. We attempted to probe and summarize molecular mechanisms for thermal stabilization of a monoclonal antibody (mAb) by developing quantitative structure-activity relationships using a rationally-selected library of 120 osmolyte-like compounds in the polyhydric alcohols, amino acids and methylamines classes. Thermal stabilization potencies were experimentally determined by thermal shift assays based on differential scanning fluorimetry. The cross-validated QSAR model was developed by partial least squares regression using descriptors generated from Molecular Operating Environment software. Careful evaluation of the results with the use of variable importance in projection parameter (VIP) and regression coefficients guided the selection of the most relevant descriptors influencing mAb thermal stability. For the mAb studied and at pH 7, the thermal stabilization effects of tested compounds correlated positively with their fractional polar surface area and inversely with their fractional hydrophobic surface area. We cannot claim that the observed trends are universal for osmolyte-protein interactions because of protein-specific effects, however this approach should guide the quick selection of (de)stabilizing compounds for a protein from a chemical library. Further work with a large variety of proteins and at different pH values would help the derivation of a solid explanation as to the nature of favorable osmolyte-protein interactions for improved thermal stability. This approach may be beneficial in the design of novel protein stabilizers with optimal property values, especially when the influence of solution conditions like the pH and buffer species and the protein properties are factored in.

Keywords: thermal stability, monoclonal antibodies, quantitative structure-activity relationships, osmolytes

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Authors: Nikkey Keshri

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Arctic is a polar region located at the north of the earth. This consists of the Arctic Ocean and other parts of Canada, Russia, the United States, Denmark, Norway, Sweden, Finland, and Iceland. Arctic has vast natural resources which are exploited with modern technology, and the economic opening up of Russia has given new opportunities. All these states have connected with the Arctic region for economic activities and this effect the region ecology. The pollution problem is a serious threat to the people health living around pollution sources. Due to the prevailing worldwide sea and air currents, the Arctic area is the fallout region for long-range transport pollutants, and in some places the concentrations exceed the levels of densely populated urban areas. The Arctic is especially vulnerable to the effects of global warming, as has become apparent in the melting sea ice in recent years. Climate models predict much greater warming in the Arctic than the global average, resulting in significant international attention to the region. The global warming has an adverse impact on the climate, indigenous people, wildlife, and infrastructure. However, there are several opportunities that have emerged in the form of shipping routes, resources, and new territories. The shipping route through the Arctic is a reality and is currently navigable for a few weeks during summers. There are large deposits of oil and gas, minerals and fish and the surrounding countries with Arctic coastlines are becoming quite assertive about exercising their sovereignty over the newfound wealth. The main part of the research is that how the opening of Northern Sea Route is providing opportunities or problem in the Arctic and it is becoming geopolitically important. It focuses on the interest Arctic and non Arctic states, their present and anticipated global geopolitical aims. The Northern Sea Route might open up due to climate changes and that Iceland might benefit or has an impact from the situation. Efforts will be made to answer the research question: ‘Whether Opening of North Sea Route is providing opportunities or becoming a risk for Arctic region?’ Every research has a structure which usually called design. In this research, both Qualitative and Quantitative method is used in terms of various literature, maps, pie- charts, etc to find out the answer for the research question. The aim of this research is to find out the impact of Opening of North Sea Route over Arctic region and how this make arctic geopolitically important. The aim behind this research is to find out the impact of climate change and how the particular geographical area is being affected.

Keywords: climate change, geopolitics, international relation, Northern Sea Route

Procedia PDF Downloads 258

Authors: Danilo A. F. Fontes, Magaly A. M.Lyra, Maria L. C. Moura, Leslie R. M. Ferraz, Salvana P. M. Costa, Amanda C. Q. M. Vieira, Larissa A. Rolim, Giovanna C. R. M. Schver, Ping I. Lee, Severino Alves-Júnior, José L. Soares-Sobrinho, Pedro J. Rolim-Neto

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Efavirenz (EFV) is a first-choice drug in antiretroviral therapy with high efficacy in the treatment of infection by Human Immunodeficiency Virus, which causes Acquired Immune Deficiency Syndrome (AIDS). EFV has low solubility in water resulting in a decrease in the dissolution rate and, consequently, in its bioavailability. Among the technological alternatives to increase solubility, the Lamellar Double Hydroxides (LDH) have been applied in the development of systems with poorly water-soluble drugs. The use of analytical techniques such as X-Ray Diffraction (XRD), Infrared Spectroscopy (IR) and Differential Scanning Calorimetry (DSC) allowed the elucidation of drug interaction with the lamellar compounds. The objective of this work was to characterize and develop the binary systems with EFV and LDH in order to increase the solubility of the drug. The LDH-CaAl was synthesized by the method of co-precipitation from salt solutions of calcium nitrate and aluminum nitrate in basic medium. The systems EFV-LDH and their physical mixtures (PM) were obtained at different concentrations (5-60% of EFV) using the solvent technique described by Takahashi & Yamaguchi (1991). The characterization of the systems and the PM’s was performed by XRD techniques, IR, DSC and dissolution test under non-sink conditions. The results showed improvements in the solubility of EFV when associated with LDH, due to a possible change in its crystal structure and formation of an amorphous material. From the DSC results, one could see that the endothermic peak at 173°C, temperature that correspond to the melting process of EFZ in the crystal form, was present in the PM results. For the EFZ-LDH systems (with 5, 10 and 30% of drug loading), this peak was not observed. XRD profiles of the PM showed well-defined peaks for EFV. Analyzing the XRD patterns of the systems, it was found that the XRD profiles of all the systems showed complete attenuation of the characteristic peaks of the crystalline form of EFZ. The IR technique showed that, in the results of the PM, there was the appearance of one band and overlap of other bands, while the IR results of the systems with 5, 10 and 30% drug loading showed the disappearance of bands and a few others with reduced intensity. The dissolution test under non-sink conditions showed that systems with 5, 10 and 30% drug loading promoted a great increase in the solubility of EFV, but the system with 10% of drug loading was the only one that could keep substantial amount of drug in solution at different pHs.

Keywords: Efavirenz, Lamellar Double Hydroxides, Pharmaceutical Techonology, Solubility

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Authors: Irene Buj-Corral, Ali Bagheri, Alejandro Dominguez-Fernandez

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In recent years, use of ceramic prostheses as an implant in some parts of body has become common. In the present study, research has focused on replacement of the acetabulum bone, which is a part of the pelvis bone. Metallic prostheses have shown some problems such as release of metal ions into patient's blood. In addition, fracture of liners and squeezing between surface of femoral head and inner surface of acetabulum have been reported. Ceramic prostheses have the advantage of low debris and high strength, although they are more difficult to be manufactured than metallic ones. Specifically, new designs try to attempt an acetabulum in which the outer surface will be porous for proliferation of cells and fixation of the prostheses by means of osteointegration, while inner surface must be smooth enough to assure that the movement between femoral head and inner surface will be carried out with on feasibility. In the present study, 3D printing technologies are used for manufacturing ceramic prostheses. In Fused Deposition Modelling (FDM) process, 3D printed plastic prostheses are obtained by means of melting of a plastic filament and subsequent deposition on a glass surface. A similar process is applied to ceramics in which ceramic powders need to be mixed with a liquid polymer before depositing them. After 3D printing, parts are subjected to a sintering process in an oven so that they can achieve final strength. In the present paper, influence of printing parameters on surface roughness 3D printed ceramic parts are presented. Three parameter full factorial design of experiments was used. Selected variables were layer height, infill and nozzle diameter. Responses were average roughness Ra and mean roughness depth Rz. Regression analysis was applied to responses in order to obtain mathematical models for responses. Results showed that surface roughness depends mainly on layer height and nozzle diameter employed, while infill was found not to be significant. In order to get low surface roughness, low layer height and low infill should be selected. As a conclusion, layer height and infill are important parameters for obtaining good surface finish in ceramic 3D printed prostheses. However, use of too low infill could lead to prostheses with low mechanical strength. Such prostheses could not be able to bear the static and dynamic charges to which they are subjected once they are implanted in the body. This issue will be addressed in further research.

Keywords: ceramic, hip prostheses, surface roughness, 3D printing

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Authors: Birute Bugelyte, Ingrida Jurkute, Vida Vickackaite

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The most complicated step of the determination of volatile compounds in complex matrices is the separation of analytes from the matrix. Traditional analyte separation methods (liquid extraction, Soxhlet extraction) require a lot of time and labour; moreover, there is a risk to lose the volatile analytes. In recent years, headspace gas chromatography has been used to determine volatile compounds. To date, traditional extraction solvents have been used in headspace gas chromatography. As a rule, such solvents are rather volatile; therefore, a large amount of solvent vapour enters into the headspace together with the analyte. Because of that, the determination sensitivity of the analyte is reduced, a huge solvent peak in the chromatogram can overlap with the peaks of the analyts. The sensitivity is also limited by the fact that the sample can’t be heated at a higher temperature than the solvent boiling point. In 2018 it was suggested to replace traditional headspace gas chromatographic solvents with non-volatile, eco-friendly, biodegradable, inexpensive, and easy to prepare deep eutectic solvents (DESs). Generally, deep eutectic solvents have low vapour pressure, a relatively wide liquid range, much lower melting point than that of any of their individual components. Those features make DESs very attractive as matrix media for application in headspace gas chromatography. Also, DESs are polar compounds, so they can be applied for microwave assisted extraction. The aim of this work was to investigate the possibility of applying deep eutectic solvents for microwave assisted extraction and headspace gas chromatographic determination of hexanal in fat-rich food. Hexanal is considered one of the most suitable indicators of lipid oxidation degree as it is the main secondary oxidation product of linoleic acid, which is one of the principal fatty acids of many edible oils. Eight hydrophilic and hydrophobic deep eutectic solvents have been synthesized, and the influence of the temperature and microwaves on their headspace gas chromatographic behaviour has been investigated. Using the most suitable DES, microwave assisted extraction conditions and headspace gas chromatographic conditions have been optimized for the determination of hexanal in potato chips. Under optimized conditions, the quality parameters of the prepared technique have been determined. The suggested technique was applied for the determination of hexanal in potato chips and other fat-rich food.

Keywords: deep eutectic solvents, headspace gas chromatography, hexanal, microwave assisted extraction

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Authors: Hamza Javar Magnier, Robin Curtis

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There have been rapid advances in the upstream processing of protein therapeutics, which has shifted the bottleneck to downstream purification and formulation. Finding liquid formulations with shelf lives of up to two years is increasingly difficult for some of the newer therapeutics, which have been engineered for activity, but their formulations are often viscous, can phase separate, and have a high propensity for irreversible aggregation1. We explore means to develop improved predictive ability from a better understanding of how protein-protein interactions on formulation conditions (pH, ionic strength, buffer type, presence of excipients) and how these impact upon the initial steps in protein self-association and aggregation. In this work, we study the initial steps in the aggregation pathways using a minimal protein model based on square-well potentials and discontinuous molecular dynamics. The effect of model parameters, including range of interaction, stiffness, chain length, and chain sequence, implies that protein models fold according to various pathways. By reducing the range of interactions, the folding- and collapse- transition come together, and follow a single-step folding pathway from the denatured to the native state2. After parameterizing the model interaction-parameters, we developed an understanding of low-temperature conformational properties and fluctuations, and the correlation to the folding transition of proteins in isolation. The model fluctuations increase with temperature. We observe a low-temperature point, below which large fluctuations are frozen out. This implies that fluctuations at low-temperature can be correlated to the folding transition at the melting temperature. Because proteins “breath” at low temperatures, defining a native-state as a single structure with conserved contacts and a fixed three-dimensional structure is misleading. Rather, we introduce a new definition of a native-state ensemble based on our understanding of the core conservation, which takes into account the native fluctuations at low temperatures. This approach permits the study of a large range of length and time scales needed to link the molecular interactions to the macroscopically observed behaviour. In addition, these models studied are parameterized by fitting to experimentally observed protein-protein interactions characterized in terms of osmotic second virial coefficients.

Keywords: protein folding, native-ensemble, conformational fluctuation, aggregation

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Authors: Ryoma Tokonami, Teruya Goto, Tatsuhiro Takahashi,

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For enhancing the mechanical property ofcarbon fiber reinforced plastic (CFRP), the surface modification of carbon fiber (CF) by multi-walled carbon nanotube (MWCNT) has received considerable attention using direct MWCNT growth on CF with a catalysis, MWCNT electrophoresis, and layer-by-layer of MWCNT with reactive polymers, etc. Among above approaches, the layer-by-layer method is the simplest process, however, the amount of MWCNTs on CF is very little, resulting in the small amount of improvement of the mechanical property of the composite. The remaining amount of MWCNT on CF after melt mixing of CF (short fiber) with thermoplastic matrix polymer was not examined clearly in the former studies. The present research aims to propose an effective layer-by-layer chemical grafting of a highly reactive oxazoline polymer, which has not been used before, and MWCNTs onto CF using the highly reactivity of oxazoline and COOH on the surface of CF and MWCNTs.With layer-by-layer method, the first uniform chemically bonded mono molecular layer on carbon fiber was formed by chemical surface reaction of carbon fiber, a reactive oxazoline polymer solution between COOH of carbon fiber and oxazoline. The second chemically bonded uniform layer of MWCNTs on the first layer was prepared through the first layer coated carbon fiber in MWCNT dispersion solution by chemical reaction between oxazoline and COOH of MWCNTs. The quantitative analysis of MWCNTs on carbon fiber was performed, showing 0.44 wt.% of MWCNTs based on carbon fiber, which is much larger amount compared with the former studies in layer-by-layer method. In addition, MWCNTs were also observed uniform coating on carbon fiber by scanning electron micrograph (SEM). Carbon fiber composites were prepared by melting mixing using polystyrene (PS) as a thermoplastic matrix because of easy removal of PS by solvent for additional analysis, resulting the 20% of enhancement of tensile strength and modulus by tensile strength test. It was confirmed bySEM the layer-by-layer structure on carbon fibers were remained after the melt mixing by removing PS with a solvent. As a conclusion, the effectiveness for the enhancement of the mechanical properties of CF(short fiber)/PS composite using the highly reactive oxazoline polymer for the first layer and MWCNT for the second layer, which act as the physical anchor, was demonstrated.

Keywords: interface, layer-by-layer, multi walled carbon nanotubes (MWCNTs), oxazoline

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Authors: Narges Shayesteh Moghaddam

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Tungsten (W), a refractory metal known for its remarkably high melting temperature, offers tremendous potential for use in challenging environments prevalent in sectors such as space exploration, defense, and nuclear industries. Additive manufacturing, especially the Laser Powder-Bed Fusion (LPBF) technique, emerges as a beneficial method for fabricating tungsten parts. This technique enables the production of intricate components while simultaneously reducing production lead times and associated costs. However, the inherent brittleness of tungsten and its tendency to crack under high-temperature conditions pose significant challenges to the manufacturing process. Our research primarily focuses on the process of rolling tungsten parts in a layer-by-layer manner in LPBF and the subsequent changes in microstructure. Our objective is not only to identify the alterations in the microstructure but also to assess their implications on the physical properties and performance of the fabricated tungsten parts. To examine these aspects, we conducted an extensive series of experiments that included the fabrication of tungsten samples through LPBF and subsequent characterization using advanced materials analysis techniques. These investigations allowed us to scrutinize shifts in various microstructural features, including, but not limited to, grain size and grain boundaries occurring during the rolling process. The results of our study provide crucial insights into how specific factors, such as plastic deformation occurring during the rolling process, influence the microstructural characteristics of the fabricated parts. This information is vital as it provides a foundation for understanding how the parameters of the layer-by-layer rolling process affect the final tungsten parts. Our research significantly broadens the current understanding of microstructural evolution in tungsten parts produced via the layer-by-layer rolling process in LPBF. The insights obtained will play a pivotal role in refining and optimizing manufacturing parameters, thus improving the mechanical properties of tungsten parts and, therefore, enhancing their performance. Furthermore, these findings will contribute to the advancement of manufacturing techniques, facilitating the wider application of tungsten parts in various high-demand sectors. Through these advancements, this research represents a significant step towards harnessing the full potential of tungsten in high-temperature and high-stress applications.

Keywords: additive manufacturing, rolling, tungsten, refractory materials

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Authors: Amit Mallik, Anil K. Barik, Biswajit Pal

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The galloping advancement of research work on glass-ceramics stems from their wide applications in electronic industry and also to some extent in application oriented medical dentistry. TiO2, even in low concentration has been found to strongly influence the physical and mechanical properties of the glasses. Glass-ceramics is a polycrystalline ceramic material produced through controlled crystallization of glasses. Crystallization is accomplished by subjecting the suitable parent glasses to a regulated heat treatment involving the nucleation and growth of crystal phases in the glass. Mica glass-ceramics is a new kind of glass-ceramics based on the system SiO2•MgO•K2O•F. The predominant crystalline phase is synthetic fluormica, named fluorophlogopite. Mica containing glass-ceramics flaunt an exceptional feature of machinability apart from their unique thermal and chemical properties. Machinability arises from the randomly oriented mica crystals with a 'house of cards' microstructures allowing cracks to propagate readily along the mica plane but hindering crack propagation across the layers. In the present study, we have systematically investigated the crystallization, microstructure and mechanical behavior of barium fluorophlogopite mica-containing glass-ceramics of composition BaO•4MgO•Al2O3•6SiO2•2MgF2 nucleated by addition of 2, 4, 6 and 8 wt% TiO2. The glass samples were prepared by the melting technique. After annealing, different batches of glass samples for nucleation were fired at 730°C (2wt% TiO2), 720°C (4 wt% TiO2), 710°C (6 wt% TiO2) and 700°C (8 wt% TiO2) batches respectively for 2 h and ultimately heated to corresponding crystallization temperatures. The glass batches were analyzed by differential thermal analysis (DTA) and x-ray diffraction (XRD), scanning electron microscopy (SEM) and micro hardness indenter. From the DTA study, it is found that the fluorophlogopite mica crystallization exotherm appeared in the temperature range 886–903°C. Glass transition temperature (Tg) and crystallization peak temperature (Tp) increased with increasing TiO2 content up to 4 wt% beyond this weight% the glass transition temperature (Tg) and crystallization peak temperature (Tp) start to decrease with increasing TiO2 content up to 8 wt%. Scanning electron microscopy confirms the development of an interconnected ‘house of cards’ microstructure promoted by TiO2 as a nucleating agent. The increase in TiO2 content decreases the vicker’s hardness values in glass-ceramics.

Keywords: crystallization, fluormica glass, ‘house of cards’ microstructure, hardness

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Authors: Han-Mei Chen, Rongxin Zhou, Taige Wang

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Glass is widely used in everyday life, from glass bottles for beverages to architectural glass for various forms of glazing. Although the mainstream of used glass is recycled in the UK, the single-use and then recycling procedure results in a lot of waste as it incorporates intact glass with smashing, re-melting, and remanufacturing. These processes bring massive energy consumption with a huge loss of high embodied energy and economic value, compared to re-use, which’s towards a ‘zero carbon’ target. As a tourism city, Liverpool has more glass bottle consumption than most less leisure-focused cities. It’s therefore vital for Liverpool to find an upgrading approach for the single-use glass bottles with low carbon output. This project aims to assess the feasibility of industrial symbiosis and upgrading the framework of glass and to investigate the ways of achieving them. It is significant to Liverpool’s future industrial strategy since it provides an opportunity to target economic recovery for post-COVID by industry symbiosis and up-grading waste management in Liverpool to respond to the climate emergency. In addition, it will influence the local government policy for glass bottle reuse and recycling in North West England and as a good practice to be further recommended to other areas of the UK. First, a critical literature review of glass waste strategies has been conducted in the UK and worldwide industrial symbiosis practices. Second, mapping, data collection, and analysis have shown the current life cycle chain and the strong links of glass reuse and upgrading potentials via site visits to 16 local waste recycling centres. The results of this research have demonstrated the understanding of the influence of key factors on the development of a circular industrial symbiosis business model for beverage glass bottles. The current waste management procedures of the glass bottle industry, its business model, supply chain, and material flow have been reviewed. The various potential opportunities for glass bottle up-valuing have been investigated towards an industrial symbiosis in Liverpool. Finally, an up-valuing business model has been developed for an industrial symbiosis framework of glass in Liverpool. For glass bottles, there are two possibilities 1) focus on upgrading processes towards re-use rather than single-use and recycling and 2) focus on ‘smart’ re-use and recycling, leading to optimised values in other sectors to create a wider industry symbiosis for a multi-level and circular economy.

Keywords: glass bottles, industry symbiosis, smart re-use, waste upgrading

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Authors: Hamid Fallah

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Undoubtedly, flood is known as a natural disaster, and in practice, flood is considered the most terrible natural disaster in the world both in terms of loss of life and financial losses. From 1988 to 1997, about 390,000 people were killed by natural disasters in the world, 58% of which were related to floods, 26% due to earthquakes, and 16% due to storms and other disasters. The total damages in these 10 years were about 700 billion dollars, which were 33, 29, 28% related to floods, storms and earthquakes, respectively. In this regard, the worrisome point has been the increasing trend of flood deaths and damages in the world in recent decades. The increase in population and assets in flood plains, changes in hydro systems and the destructive effects of human activities have been the main reasons for this increase. During rain and snow, some of the water is absorbed by the soil and plants. A percentage evaporates and the rest flows and is called runoff. Floods occur when the soil and plants cannot absorb the rainfall, and as a result, the natural river channel does not have the capacity to pass the generated runoff. On average, almost 30% of precipitation is converted into runoff, which increases with snow melting. Floods that occur differently create an area called flood plain around the river. River floods are often caused by heavy rains, which in some cases are accompanied by snow melt. A flood that flows in a river without warning or with little warning is called a flash flood. The casualties of these rapid floods that occur in small watersheds are generally more than the casualties of large river floods. Coastal areas are also subject to flooding caused by waves caused by strong storms on the surface of the oceans or waves caused by underground earthquakes. Floods not only cause damage to property and endanger the lives of humans and animals, but also leave other effects. Runoff caused by heavy rains causes soil erosion in the upstream and sedimentation problems in the downstream. The habitats of fish and other animals are often destroyed by floods. The high speed of the current increases the damage. Long-term floods stop traffic and prevent drainage and economic use of land. The supports of bridges, river banks, sewage outlets and other structures are damaged, and there is a disruption in shipping and hydropower generation. The economic losses of floods in the world are estimated at tens of billions of dollars annually.

Keywords: flood, hydrological engineering, gis, dam, small hydropower, suitablity

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Authors: Mantas Sriubas, Kristina Bockute, Darius Virbukas, Giedrius Laukaitis

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In this work, the doped TiO2 (dopants – Ca, Mg) was investigated. The comparison between the physical vapour deposition methods as electron beam vapour deposition and magnetron sputtering was performed and the structural and electrical properties of the formed thin films were investigated. Thin films were deposited on different type of substrates: SiO2, Alloy 600 (Fe-Ni-Cr) and Al2O3 substrates. The structural properties were investigated using Ambios XP-200 profilometer, scanning electron microscope (SEM) Hitachi S-3400N, X-ray energy-dispersive spectroscope (EDS) Quad 5040 (Bruker AXS Microanalysis GmbH), X-ray diffractometer (XRD) D8 Discover (Bruker AXS GmbH) with glancing angles focusing geometry in a 20 – 70° range using the Cu Kα1 λ = 0.1540562 nm radiation). The impedance spectroscopy measurements were performed using Probostat® (NorECs AS) measurement cell in the frequency range from 10-1-106 Hz under reducing and oxidizing conditions in temperature range of 200 °C to 1200 °C. The investigation of the e-beam deposited Ca and Mg doped-TiO2 thin films shows that the thin films are dense without any visible pores and cavities and the thin films grow in zone T according Barna-Adamik SZM. Substrate temperature was kept 600 °C during the deposition and Ts/Tm ≈ 0.32 (substrate temperature (Ts) and coating material melting temperature (Tm)). The surface diffusion is high however, the grain boundary migration is strongly limited at this temperature. This means that structure is inhomogeneous and the columnar structure is mostly visible in the upper part of the films. According to XRD, the increasing of the Ca dopants’ concentration increases the crystallinity of the formed thin films and the crystallites size increase linearly and Ca dopants act as prohibitors. Thin films are comprised of anatase TiO2 phase with an exception of 2 % Ca doped TiO2, where a small peak of Ca arise. In the case of Mg doped-TiO2 the intensities of the XRD peaks decreases with increasing Mg molar concentration. It means that there are less diffraction planes of the particular orientation in thin films with higher impurities concentration. Thus, the crystallinity decreases with increasing Mg concentration and Mg dopants act as inhibitors. The impedance measurements show that the dopants changed the conductivity of the formed thin films. The conductivity varies from 10-3 S/cm to 10-4 S/cm at 800 °C under wet reducing conditions. The microstructure of the magnetron sputtered thin TiO2 films is different comparing to the thin films deposited using e-beam deposition therefore influencing other structural and electrical properties.

Keywords: electrical properties, electron beam deposition, magnetron sputtering, microstructure, titanium dioxide

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Authors: Axel Thallemer, Aleksandar Kostadinov, Abel Fam, Alex Teo

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For centuries, the forming processes in nature served as a source of inspiration for both architects and designers. It seems as most human artifacts are based on ideas which stem from the observation of the biological world and its principles of growth. As a fact, in the cultural history of Homo faber, materials have been mostly used in their solid state: From hand axe to computer mouse, the principle of employing matter has not changed ever since the first creation. In the scope of history only recently and by the help of additive-generative fabrication processes through Computer Aided Design (CAD), designers were enabled to deconstruct solid artifacts into an outer skin and an internal lattice structure. The intention behind this approach is to create a new topology which reduces resources and integrates functions into an additively manufactured component. However, looking at the currently employed lattice structures, it is very clear that those lattice structure geometries have not been thoroughly designed, but rather taken out of basic-geometry libraries which are usually provided by the CAD. In the here presented study, a group of 20 industrial design students created new and unique lattice structures using natural paragons as their models. The selected natural models comprise both the animate and inanimate world, with examples ranging from the spiraling of narwhal tusks, off-shooting of mangrove roots, minimal surfaces of soap bubbles, up to the rhythmical arrangement of molecular geometry, like in the case of SiOC (Carbon-Rich Silicon Oxicarbide). This ideation process leads to a design of a geometric cell, which served as a basic module for the lattice structure, whereby the cell was created in visual analogy to its respective natural model. The spatial lattices were fabricated additively in mostly [X]3 by [Y]3 by [Z]3 units’ volumes using selective powder bed melting in polyamide with (z-axis) 50 mm and 100 µm resolution and subdued to mechanical testing of their elastic zone in a biomedical laboratory. The results demonstrate that additively manufactured lattice structures can acquire different properties when they are designed in analogy to natural models. Several of the lattices displayed the ability to store and return kinetic energy, while others revealed a structural failure which can be exploited for purposes where a controlled collapse of a structure is required. This discovery allows for various new applications of functional lattice structures within industrially created objects.

Keywords: bio-inspired, biomimetic, lattice structures, additive manufacturing

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Authors: I. Irska, S. Paszkiewicz, D. Pawlikowska, E. Piesowicz, A. Linares, T. A. Ezquerra

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Due to the number of advantages such as high tensile strength, sensitivity to hydrolytic degradation, and biocompatibility poly(lactic acid) (PLA) is one of the most common polyesters for biomedical and pharmaceutical applications. However, PLA is a rigid, brittle polymer with low heat distortion temperature and slow crystallization rate. In order to broaden the range of PLA applications, it is necessary to improve these properties. In recent years a number of new strategies have been evolved to obtain PLA-based materials with improved characteristics, including manipulation of crystallinity, plasticization, blending, and incorporation into block copolymers. Among the other methods, synthesis of aliphatic-aromatic copolyesters has been attracting considerable attention as they may combine the mechanical performance of aromatic polyesters with biodegradability known from aliphatic ones. Given the need for highly flexible biodegradable polymers, in this contribution, a series of aromatic-aliphatic based on poly(butylene terephthalate) and poly(lactic acid) (PBT-b-PLA) copolyesters exhibiting superior mechanical properties were copolymerized with an additional poly(tetramethylene oxide) (PTMO) soft block. The structure and properties of both series were characterized by means of attenuated total reflectance – Fourier transform infrared spectroscopy (ATR-FTIR), nuclear magnetic resonance spectroscopy (¹H NMR), differential scanning calorimetry (DSC), wide-angle X-ray scattering (WAXS) and dynamic mechanical, thermal analysis (DMTA). Moreover, the related changes in tensile properties have been evaluated and discussed. Lastly, the viscoelastic properties of synthesized poly(ester-ether) copolymers were investigated in detail by step cycle tensile tests. The block lengths decreased with the advance of treatment, and the block-random diblock terpolymers of (PBT-ran-PLA)-b-PTMO were obtained. DSC and DMTA analysis confirmed unambiguously that synthesized poly(ester-ether) copolymers are microphase-separated systems. The introduction of polyether co-units resulted in a decrease in crystallinity degree and melting temperature. X-ray diffraction patterns revealed that only PBT blocks are able to crystallize. The mechanical properties of (PBT-ran-PLA)-b-PTMO copolymers are a result of a unique arrangement of immiscible hard and soft blocks, providing both strength and elasticity.

Keywords: aliphatic-aromatic copolymers, multiblock copolymers, phase behavior, thermoplastic elastomers

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Authors: Ana Carolina Kogawa, Selma Gutierrez Antonio, Hérida Regina Nunes Salgado

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Rifaximin is an oral antimicrobial, gut - selective and not systemic with adverse effects compared to placebo. It is used for the treatment of hepatic encephalopathy, travelers diarrhea, irritable bowel syndrome, Clostridium difficile, ulcerative colitis and acute diarrhea. The crystalline form present in the rifaximin with minimal systemic absorption is α, being the amorphous form significantly different. Regulators are increasingly attention to polymorphisms. Polymorphs can change the form by altering the drug characteristics compromising the effectiveness and safety of the finished product. International Conference on Harmonization issued the ICH Guidance Q6A, which aim to improve the control of polymorphism in new and existing pharmaceuticals. The objective of this study was to obtain polymorphic forms of rifaximin employing recrystallization processes and characterize them by thermal analysis (thermogravimetry - TG and differential scanning calorimetry - DSC), X-ray diffraction, scanning electron microscopy and solubility test. Six polymorphic forms of rifaximin, designated I to VI were obtained by the crystallization process by evaporation of the solvent. The profiles of the TG curves obtained from polymorphic forms of rifaximin are similar to rifaximin and each other, however, the DTG are different, indicating different thermal behaviors. Melting temperature values of all the polymorphic forms were greater to that shown by the rifaximin, indicating the higher thermal stability of the obtained forms. The comparison of the diffractograms of the polymorphic forms of rifaximin with rifaximin α, β and γ constant in patent indicate that forms III, V and VI are formed by mixing polymorph β and α and form III is formed by polymorph β. The polymorphic form I is formed by polymorph β, but with a significant amount of amorphous material. Already, the polymorphic form II consists of polymorph γ, amorphous. In scanning electron microscope is possible to observe the heterogeneity of morphological characteristics of crystals of polymorphic forms among themselves and with rifaximin. The solubility of forms I and II was greater than the solubility of rifaximin, already, forms III, IV and V presented lower solubility than of rifaximin. Similarly, the bioavailability of the amorphous form of rifaximin is considered significantly higher than the form α, the polymorphic forms obtained in this work can not guarantee the excellent tolerability of the reference medicine. Therefore, studies like these are extremely important and they point to the need for greater requirements by the regulatory agencies competent about polymorphs analysis of the raw materials used in the manufacture of medicines marketed globally. These analyzes are not required in the majority of official compendia. Partnerships between industries, research centers and universities would be a viable way to consolidate researches in this area and contribute to improving the quality of solid drugs.

Keywords: electronic microscopy, polymorphism, rifaximin, solubility, X-ray diffraction

Procedia PDF Downloads 664

Authors: Phakamani Xaba, Robert Huberts, Bilainu Oboirien

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It has been over 200 years since margarine was discovered and manufactured using liquid oil, liquified hardstock oils and other oil phase & aqueous phase ingredients. Henry W. Bradley first used vegetable oils in liquid state and around 1871, since then; spreads have been traditionally manufactured using liquified oils. The main objective of this study was to develop a process method to produce spreads using spray dried hardstock fat powders as a structing fats in place of current liquid structuring fats. A high shear mixing system was used to condition the fat phase and the aqueous phase was prepared separately. Using a single scraped surface heat exchanger and pin stirrer, margarine was produced. The process method was developed for to produce spreads with 40%, 50% and 60% fat . The developed method was divided into three steps. In the first step, fat powders were conditioned by melting and dissolving them into liquid oils. The liquified portion of the oils were at 65 °C, whilst the spray dried fat powder was at 25 °C. The two were mixed using a mixing vessel at 900 rpm for 4 minutes. The rest of the ingredients i.e., lecithin, colorant, vitamins & flavours were added at ambient conditions to complete the fat/ oil phase. The water phase was prepared separately by mixing salt, water, preservative, acidifier in the mixing tank. Milk was also separately prepared by pasteurizing it at 79°C prior to feeding it into the aqueous phase. All the water phase contents were chilled to 8 °C. The oil phase and water phase were mixed in a tank, then fed into a single scraped surface heat exchanger. After the scraped surface heat exchanger, the emulsion was fed in a pin stirrer to work the formed crystals and produce margarine. The margarine produced using the developed process had fat levels of 40%, 50% and 60%. The margarine passed all the qualitative, stability, and taste assessments. The scores were 6/10, 7/10 & 7.5/10 for the 40%, 50% & 60% fat spreads, respectively. The success of the trials brought about differentiated knowledge on how to manufacture spreads using non micronized spray dried fat powders as hardstock. Manufacturers do not need to store structuring fats at 80-90°C and even high in winter, instead, they can adapt their processes to use fat powders which need to be stored at 25 °C. The developed process method used one scrape surface heat exchanger instead of the four to five currently used in votator based plants. The use of a single scraped surface heat exchanger translated to about 61% energy savings i.e., 23 kW per ton of product. Furthermore, it was found that the energy saved by implementing separate pasteurization was calculated to be 6.5 kW per ton of product produced.

Keywords: margarine emulsion, votator technology, margarine processing, scraped sur, fat powders

Procedia PDF Downloads 90

Authors: Krishna Nand, Mohammad Taufik

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Fused Filament Fabrication (FFF) is one of the most popular additive manufacturing (AM) technology. In FFF technology, a wire form material (filament) is fed inside a heated chamber, where it gets converted into semi-solid form and extruded out of a nozzle to be deposited on the build platform to fabricate the part. FFF technology is expanding and covering the market at a very rapid rate, so the need of raw materials for 3D printing is also increasing. The cost of 3D printing is directly affected by filament cost. To make 3D printing more economic, a compact and portable filament/wire extrusion system is needed. Wire extrusion systems to extrude ordinary wire/filament made of a single material are available in the market. However, extrusion system to make a composite wire/filament are not available. Hence, in this study, initial efforts have been made to develop a table-top composite wire extruder. The developed system is consisted of mechanical parts, electronics parts, and a control system. A multiple channel hopper, extrusion screw, melting chamber and nozzle, cooling zone, and spool winder are some mechanical parts. While motors, heater, temperature sensor, cooling fans are some electronics parts, which are used to develop this system. A control board has been used to control the various process parameters like – temperature and speed of motors. For the production of composite wire/filament, two different materials could be fed through two channels of hopper, which will be mixed and carried to the heated zone by extrusion screw. The extrusion screw is rotated by a motor, and the speed of this motor will be controlled by the controller as per the requirement of material extrusion rate. In the heated zone, the material will melt with the help of a heating element and extruded out of the nozzle in the form of wire. The developed system occupies less floor space due to the vertical orientation of its heating chamber. It is capable to extrude ordinary filament as well as composite filament, which are compatible with 3D printers available in the market. Further, the developed system could be employed in the research and development of materials, processing, and characterization for 3D printer. The developed system presented in this study could be a better choice for hobbyists and researchers dealing with the fused filament fabrication process to reduce the 3D printing cost significantly by recycling the waste material into 3D printer feed material. Further, it could also be explored as a better alternative for filament production at the commercial level.

Keywords: additive manufacturing, 3D Printing, filament extrusion, pellet extrusion

Procedia PDF Downloads 168

Authors: Bjorn Kierulf, Arun Chundru

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Over the past decade, collegiate rocketry teams have emerged across the country with various goals: space, liquid-fueled flight, etc. A critical piece of the development of knowledge within a club is the use of so-called "sounding rockets," whose goal is to take in-flight measurements that inform future rocket design. Common measurements include acceleration from inertial measurement units (IMU's), and altitude from barometers. With a properly tuned filter, these measurements can be used to find velocity, but are susceptible to noise, offset, and filter settings. Instead, velocity can be measured more directly and more instantaneously using a pitot tube, which operates by measuring the stagnation pressure. At supersonic speeds, an additional thermodynamic property is necessary to constrain the upstream state. One possibility is the stagnation temperature, measured by a thermocouple in the pitot tube. The routing of the pitot tube from the nosecone tip down to a pressure transducer is complicated by the nosecone's structure. Commercial-off-the-shelf (COTS) nosecones come with a removable metal tip (without a pitot tube). This provides the opportunity to make custom tips with integrated measurement systems without making the nosecone from scratch. The main design constraint is how the nosecone tip is held down onto the nosecone, using the tension in a threaded rod anchored to a bulkhead below. Because the threaded rod connects into a threaded hole in the center of the nosecone tip, the pitot tube follows a winding path, and the pressure fitting is off-center. Two designs will be presented in the paper, one with a curved pitot tube and a coaxial design that eliminates the need for the winding path by routing pressure through a structural tube. Additionally, three manufacturing methods will be presented for these designs: bound powder filament metal 3D printing, stereo-lithography (SLA) 3D printing, and traditional machining. These will employ three different materials, copper, steel, and proprietary resin. These manufacturing methods and materials are relatively low cost, thus accessible to student researchers. These designs and materials cover multiple use cases, based on how fast the sounding rocket is expected to travel and how important heating effects are - to measure and to avoid melting. This paper will include drawings showing key features and an overview of the design changes necessitated by the manufacture. It will also include a look at the successful use of these nosecone tips and the data they have gathered to date.

Keywords: additive manufacturing, machining, pitot tube, sounding rocketry

Procedia PDF Downloads 165

Authors: Syahrir Andi Mangga

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During 1989–1993, the Geological Research and Development Center (recent Geological Survey Institute) Geological Agency, Ministry of Energy and Mineral Resources Republic of Indonesia was the collaboration with British Geological Survey, the United Kingdom to do technical assistance in order to collect data of geology in Sumatra Island. The overall corporation of technical programs was larger concern in stratigraphy, geochemical and age-dating studies. Availability of new data has been stimulated to reassessment of tectonic evolution of Sumatra Island. The study area located in Southern Sumatra within at latitudes 0°-6° S and 99°40’-106’00 E longitudes. The study tectonic is situated within along South Western margin of Sunda land, The Southeast Asia Continental extension arc of the Eurasian Plate and formed as part of Sunda Arc. The oceanic crust of Indian-Australian plate recently is being oblique subduction along the Sunda Trench off the West coast Sumatra. The Mesozoic-Cenozoic of the volcanic and granitic rocks can be divided into northern and southern plutons, defining a series subparallel, controlled by fault, northwest-southeast trending belts, some of the plutons are deformed and under-formed. They are widely exposed along the south-eastern side of the Barisan mountain. Based on the characteristic of minerals and crystallography, rocks found in this study area were granite, granitic, monzogranite and andesitic-Basaltic Volcanic Rock. It belongs to calc Alkaline was predominantly metalumina, I-Type Granite, Volcanic arc granites, Syncollisonal Granites (Syn_COLG) and tholeiitic basalt. It was formed since 169±5 to 20±1 Ma. The origin of magmas in interpreted to be derived from partial melting of igneous rock. The occurrence of the gratoid and volcanic rocks supposed to be closely related to the subduction of the Australian-Hindia oceanic crust beneath the Eurasia/Sunda land Continental Crust as Volcanic arc or continental margin granitic and shown youngest to the southwest. The subduction process having probably been different in position between one terrane to others led to the occurrence of segmentation subduction system. The positional discontinuities of the subduction are probably caused by the difference in time of emplacement and mechanism of volcanic and granitic rock between segments.

Keywords: tectonic setting, I-type granitic, subduction, Southern Sumatra

Procedia PDF Downloads 246

Authors: Vanda Ferreira Ribeiro, Daiane Tomacheski, Douglas Naue Simões, Michele Pitto, Ruth Marlene Campomanes Santana

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Indoor environments, such as car cabins and public transportation vehicles are places where users are subject to air quality. Microorganisms (bacteria, fungi, yeasts) enter these environments through windows, ventilation systems and may use the organic particles present as a growth substrate. In addition, atmospheric pollutants can act as potential carbon and nitrogen sources for some microorganisms. Compounds base SEBS copolymers, poly(styrene-b-(ethylene-co-butylene)-b-styrene, are a class of thermoplastic elastomers (TPEs), fully recyclable and largely used in automotive parts. Metals, such as cooper and silver, have biocidal activities and the production of the SEBS compounds by melting blending with these agents can be a good option for producing compounds for use in plastic parts of ventilation systems and automotive air-conditioning, in order to minimize the problems caused by growth of pathogenic microorganisms. In this sense, the aim of this work was to evaluate the effect of copper microparticles as antimicrobial agent in compositions based on SEBS/PP/oil/calcite. Copper microparticles were used in weight proportion of 0%, 1%, 2% and 4%. The compounds were prepared using a co-rotating double screw extruder (L/D ratio of 40/1 and 16 mm screw diameter). The processing parameters were 300 rpm of screw rotation rate, with a temperature profile between 150 to 190°C. SEBS based TPE compounds were injection molded. The compounds emission were characterized by gravimetric fogging test. Compounds were characterized by physical (density and staining by contact), mechanical (hardness and tension properties) and rheological properties (melt volume rate – MVR). Antibacterial properties were evaluated against Staphylococcus aureus (S. aureus) and Escherichia coli (E. coli) strains. To avaluate the abilities toward the fungi have been chosen Aspergillus niger (A. niger), Candida albicans (C. albicans), Cladosporium cladosporioides (C. cladosporioides) and Penicillium chrysogenum (P. chrysogenum). The results of biological tests showed a reduction on bacteria in up to 88% in E.coli and up to 93% in S. aureus. The tests with fungi showed no conclusive results because the sample without copper also demonstrated inhibition of the development of these microorganisms. The copper addition did not cause significant variations in mechanical properties, in the MVR and the emission behavior of the compounds. The density increases with the increment of copper in compounds.

Keywords: air conditioner, antimicrobial, cooper, SEBS

Procedia PDF Downloads 282

Authors: Igor V. Savchenko, Dmitrii A. Samoshkin

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The active study of the properties of lanthanides has begun in the late 50s of the last century, when methods for their purification were developed and metals with a relatively low content of impurities were obtained. Nevertheless, up to date, many properties of the rare earth metals (REM) have not been experimentally investigated, or insufficiently studied. Currently, the thermal conductivity and thermal diffusivity of lanthanides have been studied most thoroughly in the low-temperature region and at moderate temperatures (near 293 K). In the high-temperature region, corresponding to the solid phase, data on the thermophysical characteristics of the REM are fragmentary and in some cases contradictory. Analysis of the literature showed that the data on the thermal conductivity and thermal diffusivity of light REM in the liquid state are few in number, little informative (only one point corresponds to the liquid state region), contradictory (the nature of the thermal conductivity change with temperature is not reproduced), as well as the results of measurements diverge significantly beyond the limits of the total errors. Thereby our experimental results allow to fill this gap and to clarify the existing information on the heat transfer coefficients of neodymium and samarium in a wide temperature range from the melting point up to 1770 K. The measurement of the thermal conductivity of investigated metallic melts was carried out by laser flash technique on an automated experimental setup LFA-427. Neodymium sample of brand NM-1 (99.21 wt % purity) and samarium sample of brand SmM-1 (99.94 wt % purity) were cut from metal ingots and then ones were annealed in a vacuum (1 mPa) at a temperature of 1400 K for 3 hours. Measuring cells of a special design from tantalum were used for experiments. Sealing of the cell with a sample inside it was carried out by argon-arc welding in the protective atmosphere of the glovebox. The glovebox was filled with argon with purity of 99.998 vol. %; argon was additionally cleaned up by continuous running through sponge titanium heated to 900–1000 K. The general systematic error in determining the thermal conductivity of investigated metallic melts was 2–5%. The approximation dependences and the reference tables of the thermal conductivity and thermal diffusivity coefficients were developed. New reliable experimental data on the transport properties of the REM and their changes in phase transitions can serve as a scientific basis for optimizing the industrial processes of production and use of these materials, as well as ones are of interest for the theory of thermophysical properties of substances, physics of metals, liquids and phase transformations.

Keywords: high temperatures, laser flash technique, liquid state, metallic melt, rare earth metals, thermal conductivity, thermal diffusivity

Procedia PDF Downloads 198

Authors: Kyung Jin Kim, Jiwon Kwak, Jae-Hoon Lee, Soo Suk Lee

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MicroRNAs (miRNA) are a class of endogenous, single-stranded, small, and non-protein coding RNA molecules typically 20-25 nucleotides long. They are thought to regulate the expression of other genes in a broad range by binding to 3’- untranslated regions (3’-UTRs) of specific mRNAs. The detection of miRNAs is very important for understanding of the function of these molecules and in the diagnosis of variety of human diseases. However, detection of miRNAs is very challenging because of their short length and high sequence similarities within miRNA families. So, a simple-to-use, low-cost, and highly sensitive method for the detection of miRNAs is desirable. In this study, we demonstrate a novel bi-directional extension (BDE) assay. In the first step, a specific linear RT primer is hybridized to 6-10 base pairs from the 3’-end of a target miRNA molecule and then reverse transcribed to generate a cDNA strand. After reverse transcription, the cDNA was hybridized to the 3’-end which is BDE sequence; it played role as the PCR template. The PCR template was amplified in an SYBR green-based quantitative real-time PCR. To prove the concept, we used human brain total RNA. It could be detected quantitatively in the range of seven orders of magnitude with excellent linearity and reproducibility. To evaluate the performance of BDE assay, we contrasted sensitivity and specificity of the BDE assay against a commercially available poly (A) tailing method using miRNAs for let-7e extracted from A549 human epithelial lung cancer cells. The BDE assay displayed good performance compared with a poly (A) tailing method in terms of specificity and sensitivity; the CT values differed by 2.5 and the melting curve showed a sharper than poly (A) tailing methods. We have demonstrated an innovative, cost-effective BDE assay that allows improved sensitivity and specificity in detection of miRNAs. Dynamic range of the SYBR green-based RT-qPCR for miR-145 could be represented quantitatively over a range of 7 orders of magnitude from 0.1 pg to 1.0 μg of human brain total RNA. Finally, the BDE assay for detection of miRNA species such as let-7e shows good performance compared with a poly (A) tailing method in terms of specificity and sensitivity. Thus BDE proves a simple, low cost, and highly sensitive assay for various miRNAs and should provide significant contributions in research on miRNA biology and application of disease diagnostics with miRNAs as targets.

Keywords: bi-directional extension (BDE), microRNA (miRNA), poly (A) tailing assay, reverse transcription, RT-qPCR

Procedia PDF Downloads 166

Authors: Ramin Hosseinnezhad, Iurii Vozniak, Andrzej Galeski

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Shear-induced crystallization, originated from orientation of chains along the flow direction, is an inevitable part of most polymer processing technologies. It plays a dominant role in determining the final product properties and is affected by many factors such as shear rate, cooling rate, total strain, etc. Investigation of the shear-induced crystallization process become of great importance for preparation of nanocomposite, which requires crystallization of nanofibrous sheared inclusions at higher temperatures. Thus, the effects of shear time, shear rate, and also thermal condition of cooling on crystallization of two aliphatic-aromatic copolyesters have been investigated. This was performed using Linkam optical shearing system (CSS450) for both Ecoflex® F Blend C1200 produced by BASF and synthesized copolyester of butylene terephthalate and a mixture of butylene esters: adipate, succinate, and glutarate, (PBASGT), containing 60% of aromatic comonomer. Crystallization kinetics of these biodegradable copolyesters was studied at two different conditions of shearing. First, sample with a thickness of 60µm was heated to 60˚C above its melting point and subsequently subjected to different shear rates (100–800 sec-1) while cooling with specific rates. Second, the same type of sample was cooled down when shearing at constant temperature was finished. The intensity of transmitted depolarized light, recorded by a camera attached to the optical microscope, was used as a measure to follow the crystallization. Temperature dependencies of conversion degree of samples during cooling were collected and used to determine the half-temperature (Th), at which 50% conversion degree was reached. Shearing ecoflex films for 45 seconds with a shear rate of 100 sec-1 resulted in significant increase of Th from 56˚C to 70˚C. Moreover, the temperature range for the transition of molten samples to crystallized state decreased from 42˚C to 20˚C. Comparatively low shift of 10˚C in Th towards higher temperature was observed for PBASGT films at shear rate of 600 sec-1 for 45 seconds. However, insufficient melt flow strength and non-laminar flow due to Taylor vortices was a hindrance to reach more elevated Th at very high shear rates (600–800 sec-1). The shift in Th was smaller for the samples sheared at a constant temperature and subsequently cooled down. This may be attributed to the longer time gap between cessation of shearing and the onset of crystallization. The longer this time gap, the more possibility for crystal nucleus to re-melt at temperatures above Tm and for polymer chains to recoil and relax. It is found that the crystallization temperature, crystallization induction time and spherulite growth of aliphatic-aromatic copolyesters are dramatically influenced by both the cooling rate and the shear imposed during the process.

Keywords: induced crystallization, shear rate, aliphatic-aromatic copolyester, ecoflex

Procedia PDF Downloads 448

Authors: G. Zakharov, Z. Aslamazashvili, M. Chikhradze, D. Kvaskhvadze, N. Khidasheli, S. Gvazava

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Traditional technologies for processing iron-containing industrial waste, including steel-rolling production, are associated with significant energy costs, the long duration of processes, and the need to use complex and expensive equipment. Waste generated during the industrial process negatively affects the environment, but at the same time, it is a valuable raw material and can be used to produce new marketable products. The study of the effectiveness of self-propagating high-temperature synthesis (SHS) methods, which are characterized by the simplicity of the necessary equipment, the purity of the final product, and the high processing speed, is under the wide scientific and practical interest to solve the set problem. The work presents technological aspects of the production of Ferro boron by the method of SHS - metallurgy from iron-containing wastes of rolled production for alloying of cast iron and results of the effect of alloying element on the degree of boron assimilation with liquid cast iron. Features of Fe-B system combustion have been investigated, and the main parameters to control the phase composition of synthesis products have been experimentally established. Effect of overloads on patterns of cast ligatures formation and mechanisms structure formation of SHS products was studied. It has been shown that an increase in the content of hematite Fe₂O₃ in iron-containing waste leads to an increase in the content of phase FeB and, accordingly, the amount of boron in the ligature. Boron content in ligature is within 3-14%, and the phase composition of obtained ligatures consists of Fe₂B and FeB phases. Depending on the initial composition of the wastes, the yield of the end product reaches 91 - 94%, and the extraction of boron is 70 - 88%. Combustion processes of high exothermic mixtures allow to obtain a wide range of boron-containing ligatures from industrial wastes. In view of the relatively low melting point of the obtained SHS-ligature, the positive dynamics of boron absorption by liquid iron is established. According to the obtained data, the degree of absorption of the ligature by alloying gray cast iron at 1450°C is 80-85%. When combined with the treatment of liquid cast iron with magnesium, followed by alloying with the developed ligature, boron losses are reduced by 5-7%. At that, uniform distribution of boron micro-additives in the volume of treated liquid metal is provided. Acknowledgment: This work was supported by Shota Rustaveli Georgian National Science Foundation of Georgia (SRGNSFG) under the GENIE project (grant number № CARYS-19-802).

Keywords: self-propagating high-temperature synthesis, cast iron, industrial waste, ductile iron, structure formation

Procedia PDF Downloads 123

Authors: Bina Gupta, Rashmi Singh, Harshit Mahandra

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Molybdenum is a strategic metal and finds applications in petroleum refining, thermocouples, X-ray tubes and in making of steel alloy owing to its high melting temperature and tensile strength. The growing significance and economic value of molybdenum has increased interest in the development of efficient processes aiming its recovery from secondary sources. Main secondary sources of Mo are molybdenum catalysts which are used for hydrodesulphurisation process in petrochemical refineries. The activity of these catalysts gradually decreases with time during the desulphurisation process as the catalysts get contaminated with toxic material and are dumped as waste which leads to environmental issues. In this scenario, recovery of molybdenum from spent catalyst is significant from both economic and environmental point of view. Recently ionic liquids have gained prominence due to their low vapour pressure, high thermal stability, good extraction efficiency and recycling capacity. The present study reports recovery of molybdenum from Mo-Co spent leach liquor using Cyphos IL 102[trihexyl(tetradecyl)phosphonium bromide] as an extractant. Spent catalyst was leached with 3.0 mol/L HCl, and the leach liquor containing Mo-870 ppm, Co-341 ppm, Al-508 ppm and Fe-42 ppm was subjected to extraction step. The effect of extractant concentration on the leach liquor was investigated and almost 85% extraction of Mo was achieved with 0.05 mol/L Cyphos IL 102. Results of stripping studies revealed that 2.0 mol/L HNO3 can effectively strip 94% of the extracted Mo from the loaded organic phase. McCabe- Thiele diagrams were constructed to determine the number of stages required for quantitative extraction and stripping of molybdenum and were confirmed by countercurrent simulation studies. According to McCabe- Thiele extraction and stripping isotherms, two stages are required for quantitative extraction and stripping of molybdenum at A/O= 1:1. Around 95.4% extraction of molybdenum was achieved in two-stage counter current at A/O= 1:1 with the negligible extraction of Co and Al. However, iron was coextracted and removed from the loaded organic phase by scrubbing with 0.01 mol/L HCl. Quantitative stripping (~99.5 %) of molybdenum was achieved with 2.0 mol/L HNO₃ in two stages at O/A=1:1. Overall ~95.0% molybdenum with 99 % purity was recovered from Mo-Co spent catalyst. From the strip solution, MoO₃ was obtained by crystallization followed by thermal decomposition. The product obtained after thermal decomposition was characterized by XRD, FE-SEM and EDX techniques. XRD peaks of MoO₃ correspond to molybdite Syn-MoO₃ structure. FE-SEM depicts the rod-like morphology of synthesized MoO₃. EDX analysis of MoO₃ shows 1:3 atomic percentage of molybdenum and oxygen. The synthesised MoO₃ can find application in gas sensors, electrodes of batteries, display devices, smart windows, lubricants and as a catalyst.

Keywords: cyphos Il 102, extraction, spent mo-co catalyst, recovery

Procedia PDF Downloads 172

Authors: Bina Gupta, Rashmi Singh, Harshit Mahandra

Abstract:

Molybdenum is a strategic metal and finds applications in petroleum refining, thermocouples, X-ray tubes and in making of steel alloy owing to its high melting temperature and tensile strength. The growing significance and economic value of molybdenum have increased interest in the development of efficient processes aiming its recovery from secondary sources. Main secondary sources of Mo are molybdenum catalysts which are used for hydrodesulphurisation process in petrochemical refineries. The activity of these catalysts gradually decreases with time during the desulphurisation process as the catalysts get contaminated with toxic material and are dumped as waste which leads to environmental issues. In this scenario, recovery of molybdenum from spent catalyst is significant from both economic and environmental point of view. Recently ionic liquids have gained prominence due to their low vapour pressure, high thermal stability, good extraction efficiency and recycling capacity. Present study reports recovery of molybdenum from Mo-Co spent leach liquor using Cyphos IL 102[trihexyl(tetradecyl)phosphonium bromide] as an extractant. Spent catalyst was leached with 3 mol/L HCl and the leach liquor containing Mo-870 ppm, Co-341 ppm, Al-508 ppm and Fe-42 ppm was subjected to extraction step. The effect of extractant concentration on the leach liquor was investigated and almost 85% extraction of Mo was achieved with 0.05 mol/L Cyphos IL 102. Results of stripping studies revealed that 2 mol/L HNO3 can effectively strip 94% of the extracted Mo from the loaded organic phase. McCabe-Thiele diagrams were constructed to determine the number of stages required for quantitative extraction and stripping of molybdenum and were confirmed by counter current simulation studies. According to McCabe-Thiele extraction and stripping isotherms, two stages are required for quantitative extraction and stripping of molybdenum at A/O= 1:1. Around 95.4% extraction of molybdenum was achieved in two stage counter current at A/O= 1:1 with negligible extraction of Co and Al. However, iron was coextracted and removed from the loaded organic phase by scrubbing with 0.01 mol/L HCl. Quantitative stripping (~99.5 %) of molybdenum was achieved with 2.0 mol/L HNO3 in two stages at O/A=1:1. Overall ~95.0% molybdenum with 99 % purity was recovered from Mo-Co spent catalyst. From the strip solution, MoO3 was obtained by crystallization followed by thermal decomposition. The product obtained after thermal decomposition was characterized by XRD, FE-SEM and EDX techniques. XRD peaks of MoO3correspond to molybdite Syn-MoO3 structure. FE-SEM depicts the rod like morphology of synthesized MoO3. EDX analysis of MoO3 shows 1:3 atomic percentage of molybdenum and oxygen. The synthesised MoO3 can find application in gas sensors, electrodes of batteries, display devices, smart windows, lubricants and as catalyst.

Keywords: cyphos IL 102, extraction, Mo-Co spent catalyst, recovery

Procedia PDF Downloads 268

Authors: V. Nikolov, I. Koseva, R. Sole, F. Diaz

Abstract:

Cr4+ doped oxide compounds are particularly preferred active media for solid-state lasers with a wide emission region from 1.1 to 1.6 µm. However, obtaining of single crystals of these compounds is often problematic. An alternative solution of this problem is replacing the single crystals with a transparent glassceramics containing the desired crystalline phase. Germanate compounds, especially Li2MgGeO4, Li2ZnGeO4 and Li2CaGeO4, are suitable for Cr4+ doped glass-ceramics because of their relatively low melting temperature and tetrahedral coordination of all ions. The latter ensures the presence of chromium in the 4+ valence. Cr doped Li2CaGeO4 g lass-ceramic was synthesized by thermal treating using glasses from the Li2O-CaO-GeO2-B2O3 system. Special investigations were carried out for optimizing the initial glasscomposition, as well as the thermal treated conditions. The synthesis of the glass ceramics was accompanied by appropriate characterization methods such as: XRD, TEM, EPR, UVVIS-NIR, emission spectra and time decay as main characteristic for the laser emission. From the systematic studies carried out in the four-component system Li2O-CaO-GeO2-B2O3 for establishing the Li2CaGeO4 crystallization area and suitable thermal treatment conditions, several main conclusions can be drawn: 1. The crystallization region of Li2CaGeO4 is relatively narrow, localized around the stoichiometric composition of the Li2CaGeO4 compound. 2. The presence of the glass former B2O3 strongly supports the obtaining of homogeneous glasses at relatively low temperatures, but it is also the reason for the crystallization of borate phases. 3. The crystallization of glasses during thermal treatment is related to the production of more than one phase and it is correct to speak for crystallization of a main phase and accompanying crystallization of other phases. The crystallization of a given phase is related to changing the composition of the residual glass and creating conditions for the crystallization of other phases. 4. The separate studies show that glass-ceramics with different crystallized phases in different quantitative ratios can be obtained from the same composition of glass playing by the thermal treatment conditions. In other words, the choice of temperature and time of thermal treatment of the glass is an extremely important condition, along with the optimization of the starting glass composition. As a result of the conducted research, an optimal composition of the starting glass and an optimal mode of thermal treatment were selected. Glass-ceramic with a main phase Li2CaGeO4 doped by Cr4+ was obtained. The obtained glass-ceramic possess very good properties containing up to 60 mass% of Li2CaGeO4, with an average size of nanoparticles of 20 nm and with transparency about 70 % relative to the transparency of the parent glass. The emission of the obtained glass-ceramics is in a wide range between 1050 and 1500 nm. The obtained results are the basis for further optimization of the glass-ceramic characteristics to obtain an effective laser-active medium with radiation in the 1.1-1.6 nm range.

Keywords: glass, glass-ceramics, multicomponent systems, NIR emission

Procedia PDF Downloads 19

Authors: Naresh Kumar, Radhika Sharma, A. K. Singh

Abstract:

Granites from Khanak and Devsar areas, a part of Malani Igneous Suite (MIS) were investigated for their geochemical characteristics to understand the petrogenetic aspect of the research area. Neoproterozoic rocks of MIS are well exposed in Jhunjhunu, Jodhpur, Pali, Barmer, Jalor, Jaisalmer districts of Rajasthan and Bhiwani district of Haryana and also occur at Kirana hills of Pakistan. The MIS predominantly consists of acidic volcanic with acidic plutonic (granite of various types), mafic volcanic, mafic intrusive and minor amount of pyroclasts. Based on the field and petrographical studies, 28 samples were selected and analyzed for geochemical analysis of major, trace and rare earth elements at the Wadia Institute of Himalayan Geology, Dehradun by X-Ray Fluorescence Spectrometer (XRF) and ICP-MS (Inductively Coupled Plasma- Mass Spectrometry). Granites from the studied areas are categorized as grey, green and pink. Khanak granites consist of quartz, k-feldspar, plagioclase, and biotite as essential minerals and hematite, zircon, annite, monazite & rutile as accessory minerals. In Devsar granites, plagioclase is replaced by perthite and occurs as dominantly. Geochemically, granites from Khanak and Devsar areas exhibit typical A-type granites characteristics with their enrichment in SiO2, Na2O+K2O, Fe/Mg, Rb, Zr, Y, Th, U, REE (except Eu) and significant depletion in MgO, CaO, Sr, P, Ti, Ni, Cr, V and Eu suggested about A-type affinities in Northwestern Peninsular India. The amount of heat production (HP) in green and grey granites of Devsar area varies upto 9.68 & 11.70 μWm-3 and total heat generation unit (HGU) i.e. 23.04 & 27.86 respectively. Pink granites of Khanak area display a higher enrichment of HP (16.53 μWm-3) and HGU (39.37) than the granites from Devsar area. Overall, they have much higher values of HP and HGU than the average value of continental crust (3.8 HGU), which imply a possible linear relationship among the surface heat flow and crustal heat generation in the rocks of MIS. Chondrite-normalized REE patterns show enriched LREE, moderate to strong negative Eu anomalies and more or less flat heavy REE. In primitive mantle-normalized multi-element variation diagrams, the granites show pronounced depletions in the high-field-strength elements (HFSE) Nb, Zr, Sr, P, and Ti. Geochemical characteristics (major, trace and REE) along with the use of various discrimination schemes revealed their probable correspondence to magma derived from the crustal origin by a different degree of partial melting.

Keywords: A-type granite, neoproterozoic, Malani igneous suite, Khanak, Devsar

Procedia PDF Downloads 272

Authors: Chen Yuan, Nick Green, Stuart Blackburn

Abstract:

The investment casting process offers a great freedom of design combined with the economic advantage of near net shape manufacturing. It is widely used for the production of high value precision cast parts in particularly in the aerospace sector. Various combinations of materials have been used to produce the ceramic moulds, but most investment foundries use a silica based binder system in conjunction with fused silica, zircon, and alumino-silicate refractories as both filler and coarse stucco materials. However, in the context of advancing alloy technologies, silica based systems are struggling to keep pace, especially when net-shape casting titanium alloys. Study has shown that the casting of titanium based alloys presents considerable problems, including the extensive interactions between the metal and refractory, and the majority of metal-mould interaction is due to reduction of silica, present as binder and filler phases, by titanium in the molten state. Cleaner, more refractory systems are being devised to accommodate these changes. Although yttria has excellent chemical inertness to titanium alloy, it is not very practical in a production environment combining high material cost, short slurry life, and poor sintering properties. There needs to be a cost effective solution to these issues. With limited options for using pure oxides, in this work, a silica-free magnesia spinel MgAl₂O₄ was used as a primary coat filler and alumina as a binder material to produce facecoat in the investment casting mould. A comparison system was also studied with a fraction of the rare earth oxide Y₂O₃ adding into the filler to increase the inertness. The stability of the MgAl₂O₄/Al₂O₃ and MgAl₂O₄/Y₂O₃/Al₂O₃ slurries was assessed by tests, including pH, viscosity, zeta-potential and plate weight measurement, and mould properties such as friability were also measured. The interaction between the face coat and titanium alloy was studied by both a flash re-melting technique and a centrifugal investment casting method. The interaction products between metal and mould were characterized using x-ray diffraction (XRD), scanning electron microscopy (SEM) and Energy Dispersive X-Ray Spectroscopy (EDS). The depth of the oxygen hardened layer was evaluated by micro hardness measurement. Results reveal that introducing a fraction of Y₂O₃ into magnesia spinel can significantly increase the slurry life and reduce the thickness of hardened layer during centrifugal casting.

Keywords: titanium alloy, mould, MgAl₂O₄, Y₂O₃, interaction, investment casting

Procedia PDF Downloads 113

Authors: J. R. Büttler, T. Pham

Abstract:

Basic understanding of interfacial mechanisms is of importance for the development of polymer composites. For this purpose, we need techniques to analyze the quality of interphases, their chemical and physical interactions and their strength and fracture resistance. In order to investigate the interfacial phenomena in detail, advanced characterization techniques are favorable. Dynamic mechanical thermal analysis (DMTA) using a rheological system is a sensitive tool. T-peel tests were performed with this system, to investigate the temperature-dependent peel behavior of woven textile composites. A model system was made of polyamide (PA) woven fabric laminated with films of polypropylene (PP) or PP modified by grafting with maleic anhydride (PP-g-MAH). Firstly, control measurements were performed with solely PP matrixes. Polymer melt investigations, as well as the extensional stress, extensional viscosity and extensional relaxation modulus at -10°C, 100 °C and 170 °C, demonstrate similar viscoelastic behavior for films made of PP-g-MAH and its non-modified PP-control. Frequency sweeps have shown that PP-g-MAH has a zero phase viscosity of around 1600 Pa·s and PP-control has a similar zero phase viscosity of 1345 Pa·s. Also, the gelation points are similar at 2.42*104 Pa (118 rad/s) and 2.81*104 Pa (161 rad/s) for PP-control and PP-g-MAH, respectively. Secondly, the textile composite was analyzed. The extensional stress of PA66 fabric laminated with either PP-control or PP-g-MAH at -10 °C, 25 °C and 170 °C for strain rates of 0.001 – 1 s^-1 was investigated. The laminates containing the modified PP need more stress for T-peeling. However, the strengthening effect due to the modification decreases by increasing temperature and at 170 °C, just above the melting temperature of the matrix, the difference disappears. Independent of the matrix used in the textile composite, there is a decrease of extensional stress by increasing temperature. It appears that the more viscous is the matrix, the weaker the laminar adhesion. Possibly, the measurement is influenced by the fact that the laminate becomes stiffer at lower temperatures. Adhesive lap-shear testing at room temperature supports the findings obtained with the T-peel test. Additional analysis of the textile composite at the microscopic level ensures that the fibers are well embedded in the matrix. Atomic force microscopy (AFM) imaging of a cross section of the composite shows no gaps between the fibers and matrix. Measurements of the water contact angle show that the MAH grafted PP is more polar than the virgin-PP, and that suggests a more favorable chemical interaction of PP-g-MAH with PA, compared to the non-modified PP. In fact, this study indicates that T-peel testing by DMTA is a technique to achieve more insights into polymeric textile composites.

Keywords: dynamic mechanical thermal analysis, interphase, polyamide, polypropylene, textile composite

Procedia PDF Downloads 129