Search results for: microstructural characterisation

Authors: A. González-Caro, A. M. Merino-Lechuga, D. Suescum-Morales, E. Fernández-Ledesma, J. R. Jiménez, J. M. Fernández-Rodríguez

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Climate change is one of the most significant issues today. Since the 19th century, the rise in temperature has not only been due to natural change, but also to human activities, which have been the main cause of climate change, mainly due to the burning of fossil fuels such as coal, oil and gas. The boom in the construction sector in recent years is also one of the main contributors to CO₂ emissions into the atmosphere; for example, for every tonne of cement produced, 1 tonne of CO₂ is emitted into the atmosphere. Most of the research being carried out in this sector is focused on reducing the large environmental impact generated during the manufacturing process of building materials. In detail, this research focuses on the recovery of waste from olive oil mills. Spain is the world's largest producer of olive oil, and this sector generates a large amount of waste and by-products such as olive pits, “alpechín” or “alpeorujo”. This olive stone by means of a pyrosilisis process gives rise to the production of active carbon. The process causes the carbon to develop many internal spaces. This study is based on the manufacture of porous mortars with Portland cement and natural limestone sand, with an addition of 5% and 10% of activated carbon. Two curing environments were used: i) dry chamber, with a humidity of 65 ± 10% and temperature of 21 ± 2 ºC and an atmospheric CO₂ concentration (approximately 0.04%); ii) accelerated carbonation chamber, with a humidity of 65 ± 10% and temperature of 21 ± 2 ºC and an atmospheric CO₂ concentration of 5%. In addition to eliminating waste from an industry, the aim of this study is to reduce atmospheric CO₂. For this purpose, first, a physicochemical and mineralogical characterisation of all raw materials was carried out, using techniques such as fluorescence and X-ray diffraction. The particle size and specific surface area of the activated carbon were determined. Subsequently, tests were carried out on the hardened mortar, such as thermogravimetric analysis (to determine the percentage of CO₂ capture), as well as mechanical properties, density, porosity, and water absorption. It was concluded that the activated carbon acts as a sink for CO₂, causing it to be trapped inside the voids. This increases CO₂ capture by 300% with the addition of 10% activated carbon at 7 days of curing. There was an increase in compressive strength of 17.5% with the CO₂ chamber after 7 days of curing using 10% activated carbon compared to the dry chamber.

Keywords: olive stone, activated carbon, porous mortar, CO₂ capture, economy circular

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Authors: Jitendra Pratap, Jonathan Sivyer

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Introduction: Dual energy/Spectral CT scanning permits simultaneous acquisition of two x-ray spectra datasets and can complement radiological diagnosis by allowing tissue characterisation (e.g., uric acid vs. non-uric acid renal stones), enhancing structures (e.g. boost iodine signal to improve contrast resolution), and quantifying substances (e.g. iodine density). However, the latter showed inconsistent results between the 2 main modes of dual energy scanning (i.e. dual source vs. dual layer). Therefore, the present study aimed to determine which technology is more accurate in quantifying iodine density. Methods: Twenty vials with known concentrations of iodine solutions were made using Optiray 350 contrast media diluted in sterile water. The concentration of iodine utilised ranged from 0.1 mg/ml to 1.0mg/ml in 0.1mg/ml increments, 1.5 mg/ml to 4.5 mg/ml in 0.5mg/ml increments followed by further concentrations at 5.0 mg/ml, 7mg/ml, 10 mg/ml and 15mg/ml. The vials were scanned using Dual Energy scan mode on a Siemens Somatom Force at 80kV/Sn150kV and 100kV/Sn150kV kilovoltage pairing. The same vials were scanned using Spectral scan mode on a Philips iQon at 120kVp and 140kVp. The images were reconstructed at 5mm thickness and 5mm increment using Br40 kernel on the Siemens Force and B Filter on Philips iQon. Post-processing of the Dual Energy data was performed on vendor-specific Siemens Syngo VIA (VB40) and Philips Intellispace Portal (Ver. 12) for the Spectral data. For each vial and scan mode, the iodine concentration was measured by placing an ROI in the coronal plane. Intraclass correlation analysis was performed on both datasets. Results: The iodine concentrations were reproduced with a high degree of accuracy for Dual Layer CT scanner. Although the Dual Source images showed a greater degree of deviation in measured iodine density for all vials, the dataset acquired at 80kV/Sn150kV had a higher accuracy. Conclusion: Spectral CT scanning by the dual layer technique has higher accuracy for quantitative measurements of iodine density compared to the dual source technique.

Keywords: CT, iodine density, spectral, dual-energy

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Authors: H. Chabalala, A. Grootboom, M. Tang

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The innovative development, production, and clinical utilisation of African natural medicines requires frameworks from systematisation, innovation, registration. Afrika faces challenges when it comes to these sectors. The opposite is the case as is is evident in ancient Asian (Traditional Chinese Medicine and Indian Ayurveda and Siddha) medical systems, which are interfaced into their respective national health and educational systems. Afrikan Natural Medicines (ANMs) are yet to develop systematisation frameworks, i.e. disease characterisation and medicines classification. This paper explores classical medical systems drawn from Afrikan and Chinese experts in natural medicines. An Afrikological research methodology was used to conduct in-depth interviews with 20 key respondents selected through purposeful sampling technique. Data was summarised into systematisation frameworks for classical disease theories, patient categorisation, medicine classification, aetiology and pathogenesis of disease, diagnosis and prognosis techniques and treatment methods. It was discovered that ancient Afrika had systematic medical cosmologies, remnants of which are evident in most Afrikan cultural health practices. Parallels could be drawn from classical medical concepts of antiquity, like Chinese Taoist and Indian tantric health systems. Data revealed that both the ancient and contemporary ANM systems were based on living medical cosmologies. The study showed that African Natural Healing Systems have etiological systems, general pathogenesis knowledge, differential diagnostic techniques, comprehensive prognosis and holistic treatment regimes. Systematisation models were developed out of these frameworks, and this could be used for evaluation of clinical research, medical application including development of curriculum for high-education. It was envisaged that frameworks will pave way towards the development, production and commercialisation of ANMs. This was piloted in inclusive innovation, technology transfer and commercialisation of South African natural medicines, cosmeceuticals, nutraceuticals and health infusions. The central model presented here in will assist in curriculum development and establishment of Afrikan Medicines Hospitals and Pharmaceutical Industries.

Keywords: African Natural Medicines, Indigenous Knowledge Systems, Medical Cosmology, Clinical Application

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Authors: L.L. Costa, A. M. G. Brito, S. Khan, L. Schaeffer

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Microstructure resulting from the forging process is studied as a function of variables such as temperature, deformation, austenite grain size and cooling rate. The purpose of this work is to study the thermomechanical behavior of DIN 42CrMo4 (AISI 4140) steel maintained at the temperatures of 900°, 1000°, 1100° and 1200°C for the austenization times of 22, 66 and 200 minutes each and subsequently forged. These samples were quenched in water in order to study the austenite grain and to investigate the microstructure instead of quenching the annealed samples after forging they were cooled down naturally in the air. The morphologies and properties of the materials such as hardness; prepared by these two different routes have been compared. In addition to the forging experiments, the numerical simulation using the finite element model (FEM), microhardness profiles and metallography images have been presented. Forging force vs position curves has been compared with metallographic results for each annealing condition. The microstructural phenomena resulting from the hot conformation proved that longer austenization time and higher temperature decrease the forging force in the curves. The complete recrystallization phenomenon (static, dynamic and meta dynamic) was observed at the highest temperature and longest time i.e., the samples austenized for 200 minutes at 1200ºC. However, higher hardness of the quenched samples was obtained when the temperature was 900ºC for 66 minutes. The phases observed in naturally cooled samples were exclusively ferrite and perlite, but the continuous cooling diagram indicates the presence of austenite and bainite. The morphology of the phases of naturally cooled samples has shown that the phase arrangement and the previous austenitic grain size are the reasons to high hardness in obtained samples when temperature were 900ºC and 1100ºC austenization times of 22 and 66 minutes, respectively.

Keywords: austenization time, thermomechanical effects, forging process, steel AISI 4140

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Authors: Harsha B. R., K. S. Anil Kumar

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Land characterization, classification, and soil suitability evaluation of grapes-growing pedons were assessed at fifteen taluks covering four agro climatic zones of Karnataka. Study on problems and potentials of grapes cultivation in selected agro-climatic zones was carried out along with the plant sample analysis. Twenty soil profiles were excavated as study site based on the dominance of area falling under grapes production and existing spatial variability of soils. The detailed information of profiles and horizon wise soil samples were collected to study the morphological, physical, chemical, and fertility characteristics. Climatic analysis and water retention characteristics of soils of major grapes-growing areas were also done. Based on the characterisation and classification study, it was revealed that soils of Doddaballapur (Bangalore Blue and Wine grapes), Bangalore North (GKVK Farm, Rajankunte, and IIHR Farm), Devanahalli, Magadi, Hoskote, Chikkaballapur (Dilkush and Red globe), Yelaburga, Hagari Bommanahalli, Bagalkot (UHS farm) and Indi fall under the soil order Alfisol. Vijaypur pedon of northern dry zone was keyed out as Vertisols whereas, Jamkhandi and Athani as Inceptisols. Properties of Aridisols were observed in B. Bagewadi (Manikchaman and Thompson Seedless) and Afzalpur. Soil fertility status and its mapping using GIS technique revealed that all the nutrients were found to be in adequate range except nitrogen, potassium, zinc, iron, and boron, which indicated the need for application along with organic matter to improve the SOC status. Varieties differed among themselves in yield and plant nutrient composition depending on their age, climatic, soil, and management requirements. Bangalore North (GKVK farm) and Jamkhandi are having medium soil organic carbon stocks of 6.21 and 6.55 kg m⁻³, respectively. Soils of Bangalore North (Rajankunte) were highly suitable (S1) for grapes cultivation. Under northern Karnataka, Vijayapura, B. Bagewadi, Indi, and Afzalpur vineyards were good performers despite the limitations of fertility and free lime content.

Keywords: land characterization, suitability, soil orders, soil organic carbon stock

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Authors: Saeedeh Imani Moqadam, Ilya Bobrov, Jérémy Epp, Nils Ellendt, Lutz Mädler

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High entropy alloys (HEAs), having adjustable properties and enhanced stability compared with intermetallic compounds, are solid solution alloys that contain more than five principal elements with almost equal atomic percentage. The concept of producing such alloys pave the way for developing advanced materials with unique properties. However, the synthesis of such alloys may require advanced processes with high cooling rates depending on which alloy elements are used. In this study, the micro spheres of different diameters of HEAs were generated via a drop-on-demand droplet generator and subsequently solidified during free-fall in an argon atmosphere. Such droplet generators can generate individual droplets with high reproducibility regarding droplet diameter, trajectory and cooling while avoiding any interparticle momentum or thermal coupling. Metallography as well as X-ray diffraction investigations for each diameter of the generated metallic droplets where then carried out to obtain information about the microstructural state. To calculate the cooling rate of the droplets, a droplet cooling model was developed and validated using model alloys such as CuSn%6 and AlCu%4.5 for which a correlation of secondary dendrite arm spacing (SDAS) and cooling rate is well-known. Droplets were generated from these alloys and their SDAS was determined using quantitative metallography. The cooling rate was then determined from the SDAS and used to validate the cooling rates obtained from the droplet cooling model. The application of that model on the HEA then leads to the cooling rate dependency and hence to the identification of process windows for the synthesis of these alloys. These process windows were then compared with cooling rates obtained in processes such as powder production, spray forming, selective laser melting and casting to predict if a synthesis is possible with these processes.

Keywords: cooling rate, drop-on-demand, high entropy alloys, microstructure, single droplet generation, X-ray Diffractometry

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Authors: Mario Alejandro Grisales, M. Daniela Chimá, Gilberto Bejarano Gaitán

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High entropy alloys (HEA) and nitride (HEN) are currently very attractive to the automotive, aerospace, metalworking and materials forming manufacturing industry, among others, for exhibiting higher mechanical properties, wear resistance, and thermal stability than binary and ternary alloys. In this work medium-entropy coatings of TiTaZrNb and the nitrides of (TiTaZrNb)Nx were synthesized on to AISI 420 and M2 steel samples by the direct current magnetron sputtering technique. The influence of the bias voltage supplied to the substrate on the microstructure, chemical- and phase composition of the matrix coating was evaluated, and the effect of nitrogen flow on the microstructural, mechanical and tribological properties of the corresponding nitrides was studied. A change in the crystalline structure from BCC for TiTaZrNb coatings to FCC for (TiTaZrNb)Nx was observed, that is associated with the incorporation of nitrogen into the matrix and the consequent formation of a solid solution of (TiTaZrNb)Nx. An increase in hardness and residual stresses was observed with increasing bias voltage for TiTaZrNb, reaching 12.8 GPa for the coating deposited with a bias of -130V. In the case of (TiTaZrNb)Nx nitride, a greater hardness of 23 GPa is achieved for the coating deposited with a N2 flow of 12 sccm, which slightly drops to 21.7 GPa for that deposited with N2 flow of 15 sccm. The slight reduction in hardness could be associated with the precipitation of the TiN and ZrN phases that are formed at higher nitrogen flows. The specific wear rate of the deposited coatings ranged between 0.5xexp13 and 0.6xexp13 N/m2. The steel substrate exhibited an average hardness of 2.0 GPa and a specific wear rate of 203.2exp13 N/m2. Both the hardness and the specific wear rate of the synthesized nitride coatings were higher than that of the steel substrate, showing a protective effect of the steel against wear.

Keywords: medium entropy coatings, hard coatings, magnetron sputtering, tribology, wear resistance

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Authors: Ricardo Paiva, Rui Soares, Felix Harnau, Bruno Fragoso

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Nickel-based alloys are materials well suited for service in extreme environments subjected to pressure and heat. Some industrial applications for Nickel-based alloys are aerospace and jet engines, oil and gas extraction, pollution control and waste processing, automotive and marine industry. It is generally recognized that grain refinement is an effective methodology to improve the quality of casted parts. Conventional grain refinement techniques involve the addition of inoculation substances, the control of solidification conditions, or thermomechanical treatment with recrystallization. However, such methods often lead to non-uniform grain size distribution and the formation of hard phases, which are detrimental to both wear performance and biocompatibility. Stirring of the melt by electromagnetic fields has been widely used in continuous castings with success for grain refinement, solute redistribution, and surface quality improvement. Despite the advantages, much attention has not been paid yet to the use of this approach on functional castings such as investment casting. Furthermore, the effect of electromagnetic stirring (EMS) fields on Nickel-based alloys is not known. In line with the gaps/needs of the state-of-art, the present research work targets to promote new advances in controlling grain size and morphology of investment cast Nickel based alloys. For such a purpose, a set of experimental tests was conducted. A high-frequency induction furnace with vacuum and controlled atmosphere was used to cast the Inconel 718 alloy in ceramic shells. A coil surrounded the casting chamber in order to induce electromagnetic stirring during solidification. Aiming to assess the effect of the electromagnetic stirring on Ni alloys, the samples were subjected to microstructural analysis and mechanical tests. The results show that electromagnetic stirring can be an effective methodology to modify the grain size and mechanical properties of investment-cast parts.

Keywords: investment casting, grain refinement, electromagnetic stirring, nickel alloys

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Authors: Wenbo Yu, Zihao Yuan, Zhipeng Guo, Shoumei Xiong

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Under different slow shot speeds in vacuum assisted high pressure die casting (VHPDC) process, plate-shaped specimens of hypereutectic A390 aluminum alloy were produced. According to the results, the vacuum pressure inside the die cavity increased linearly with the increasing slow shot speed at the beginning of mold filling. Meanwhile, it was found that the tensile properties of vacuum die castings were deteriorated by the porosity content. In addition, the average primary Si size varies between 14µm to 23µm, which has a binary functional relationship with the slow shot speeds. Due to the vacuum effect, the castings were treated by T6 heat treatment. After heat treatment, microstructural morphologies revealed that needle-shaped and thin-flaked eutectic Si particles became rounded while Al2Cu dissolved into α-Al matrix. For the as-received sample in-situ tensile test, microcracks firstly initiate at the primary Si particles and propagated along Al matrix with a transgranular fracture mode. In contrast, for the treated sample, the crack initiated at the Al2Cu particles and propagated along Al grain boundaries with an intergranular fracture mode. In-situ three bending test, microcracks firstly formed in the primary Si particles for both samples. Subsequently, the cracks between primary Si linked along Al grain boundaries in as received sample. In contrast, the cracks in primary Si linked through the solid lines in Al matrix. Furthermore, the fractography revealed that the fracture mechanism has evolved from brittle transgranular fracture to a fracture mode with many dimples after heat treatment.

Keywords: A390 aluminum, vacuum assisted high pressure die casting, heat treatment, mechanical properties

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Authors: Xiping Guo, Fanglin Ge, Ping Guan

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Refractory high entropy alloys are alternative materials expected to be employed at high temperatures. The comprehensive changes of microstructure and properties of NbTiZrCrAl refractory high entropy alloys are systematically studied by adjusting Al content. Five kinds of button alloy ingots with different contents of Al in NbTiZrCrAlX (X=0, 0.2, 0.5, 0.75, 1.0) were prepared by vacuum non-consumable arc melting technology. The microstructure analysis results show that the five alloys are composed of BCC solid solution phase rich in Nb and Ti and Laves phase rich in Cr, Zr, and Al. The addition of Al changes the structure from hypoeutectic to hypereutectic, increases the proportion of Laves phase, and changes the structure from cubic C15 to hexagonal C14. The hardness and fracture toughness of the five alloys were tested at room temperature, and the compressive mechanical properties were tested at 1000℃. The results showed that the addition of Al increased the proportion of Laves phase and decreased the proportion of the BCC phase, thus increasing the hardness and decreasing the fracture toughness at room temperature. However, at 1000℃, the strength of 0.5Al and 0.75Al alloys whose composition is close to the eutectic point is the best, which indicates that the eutectic structure is of great significance for the improvement of high temperature strength of NbTiZrCrAl refractory high entropy alloys. The five alloys were oxidized for 1 h and 20 h in static air at 1000℃. The results show that only the oxide film of 0Al alloy falls off after oxidizing for 1 h at 1000℃. After 20h, the oxide film of all the alloys fell off, but the oxide film of alloys containing Al was more dense and complete. By producing protective oxide Al₂O₃, inhibiting the preferential oxidation of Zr, promoting the preferential oxidation of Ti, and combination of Cr₂O₃ and Nb₂O₅ to form CrNbO₄, Al significantly improves the high temperature oxidation resistance of NbTiZrCrAl refractory high entropy alloys.

Keywords: NbTiZrCrAl, refractory high entropy alloy, al content, microstructural evolution, room temperature mechanical properties, high temperature compressive strength, oxidation resistance

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Authors: Maurício N. Kleinberg, Ana P. R. N. Barroso, Frederico R. Silva, Natasha l. Gomes, Rodrigo F. Guimarães, Marcelo M. V. Parente, Jackson Q. Malveira

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Increased production of biofuels, especially biodiesel, as an option to replace the diesel derived from oil is already a reality in countries seeking a renewable and environmentally friendly fuel, as is the case in Brazil. However, it is known that the use of fuels, renewable or not, implies that it is in contact with various metallic materials which may cause corrosion. In the search for more corrosion resistant materials has been experimentally observed that the addition of molybdenum in ferritic steels increases their protective character without significantly burdening the cost of production. In order to evaluate the effect of adding molybdenum, samples of commercial steel (austenitic, ferritic and carbon steel) and the experimental ferritic alloy with a high molybdenum content (5.3%) were immersed separately into biodiesel derived from transesterification of soy oil to monitor the corrosion process of these metal samples, and in parallel to analyze the oxidative degradation of biodiesel itself. During the immersion time of 258 days, biodiesel samples were taken for analysis of acidity, kinematic viscosity, density and refraction. Likewise, the metal samples were taken from the biodiesel to be weighed and microstructurally analyzed by light microscopy. The results obtained at the end of 258 days shown that biodiesel presented a considerable increase on the values of the studied parameters for all the samples. However, this increase was not able to produce significant mass loss in metallic samples. As regards the microstructural analysis, it showed the onset of surface oxidation on the carbon steel sample. As for the other samples, no significant surface changes were shown. These results are consistent with literature for short immersion times. It is concluded that the increase in the values of the studied parameters is not significant yet, probably due to the low time of immersion and exposure of the samples. Thus, it is necessary to continue the tests so that the objectives of this work are achieved.

Keywords: biodiesel, corrosion, immersion, experimental alloy

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Authors: Yun Chen, David Penton, Fazlul Karim, Santosh Aryal, Shahriar Wahid, Peter Taylor, Susan M. Cuddy

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Droughts have severely affected Afghanistan over the last four decades, leading to critical food shortages where two-thirds of the country’s population are in a food crisis. Long years of conflict have lowered the country’s ability to deal with hazards such as drought, which can rapidly escalate into disasters. Understanding the spatial and temporal distribution of droughts is needed to be able to respond effectively to disasters and plan for future occurrences. This study used Standardized Precipitation Evapotranspiration Index (SPEI) at monthly, seasonal, and annual temporal scales to map the spatiotemporal change dynamics of drought characteristics (distribution, frequency, duration, and severity) in Afghanistan. SPEI indices were mapped for river basins, disaggregated into 189 sub-catchments, using monthly precipitation and potential evapotranspiration derived from temperature station observations from 1980 to 2017. The results show these multi-dimensional drought characteristics vary along different years, change among sub-catchments, and differ across temporal scales. During the 38 years, the driest decade and period are the 2000s and 1999–2022, respectively. The 2000–01 water year is the driest, with the whole country experiencing ‘severe’ to ‘extreme’ drought, more than 53% (87 sub-catchments) suffering the worst drought in history, and about 58% (94 sub-catchments) having ‘very frequent’ drought (7 to 8 months) or ‘extremely frequent’ drought (9 to 10 months). The estimated seasonal duration and severity present significant variations across the study area and throughout the study period. The nation also suffered from recurring droughts with varying length and intensity in 2004, 2006, 2008, and, most recently, 2011. There is a trend towards increasing drought with longer duration and higher severity extending all over sub-catchments from southeast to north and central regions. These datasets and maps help to fill the knowledge gap on detailed sub-catchment scale meteorological drought characteristics in Afghanistan. The study findings improve our understanding of the influences of climate change on drought dynamics and can guide catchment planning for reliable adaptation to and mitigation against future droughts.

Keywords: SPEI, precipitation, evapotranspiration, climate extremes

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Authors: B. J. Babalola, M. B. Shongwe

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Spark Plasma Sintering technique is a novel processing method that produces limited grain growth and highly dense variety of materials; alloys, superalloys, and carbides just to mention a few. However, initial particle size and spark plasma sintering parameters are factors which influence the grain growth and mechanical properties of sintered materials. Ni-Cr alloys are regarded as the most promising alloys for aerospace turbine blades, owing to the fact that they meet the basic requirements of desirable mechanical strength at high temperatures and good resistance to oxidation. The conventional method of producing this alloy often results in excessive grain growth and porosity levels that are detrimental to its mechanical properties. The effect of sintering temperature was evaluated on the microstructure and mechanical properties of the nanostructured Ni-17Cr alloy. Nickel and chromium powder were milled using high energy ball milling independently for 30 hours, milling speed of 400 revs/min and ball to powder ratio (BPR) of 10:1. The milled powders were mixed in the composition of Nickel having 83 wt % and chromium, 17 wt %. This was sintered at varied temperatures from 800°C, 900°C, 1000°C, 1100°C and 1200°C. The structural characteristics such as porosity, grain size, fracture surface and hardness were analyzed by scan electron microscopy and X-ray diffraction, Archimedes densitometry, micro-hardness tester. The corresponding results indicated an increase in the densification and hardness property of the alloy as the temperature increases. The residual porosity of the alloy reduces with respect to the sintering temperature and in contrast, the grain size was enhanced. The study of the mechanical properties, including hardness, densification shows that optimum properties were obtained for the sintering temperature of 1100°C. The advantages of high sinterability of Ni-17Cr alloy using milled powders and microstructural details were discussed.

Keywords: densification, grain growth, milling, nanostructured materials, sintering temperature

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Authors: Lota Largavista

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This study entitled, ‘The Organizational Structure, Development Features, and Metadiscoursal Elements in the Expository Writing of Freshman College Writers’ aimed to examine essays written by college students. It seeks to examine the organizational structure and development features of the essays and describe their defining characteristics, the linguistic elements at both macrostructural and microstructural discourse levels and the types of textual and interpersonal metadiscourse markers that are employed in order to negotiate meanings with their prospective readers. The different frameworks used to analyze the essays include Toulmin’s ( 1984) model for argument structure, Olson’s ( 2003) three-part essay structure; Halliday and Matthiesen (2004) in Herriman (2011) notions of thematic structure, Danes (1974) thematic progression or method of development, Halliday’s (2004) concept of grammatical and lexical cohesion ;Hyland’s (2005) metadiscourse strategies; and Chung and Nation’s( 2003) four-step scale for technical vocabulary. This descriptive study analyzes qualitatively and quantitatively how freshman students generally express their written compositions. Coding of units is done to determine what linguistic features are present in the essays. Findings revealed that students’ expository essays observe a three-part structure having all three moves, the Introduction, the Body and the Conclusion. Stance assertion, stance support, and emerging moves/strategies are found to be employed in the essays. Students have more marked themes on the essays and also prefer constant theme progression as their method of development. The analysis of salient linguistic elements reveals frequently used cohesive devices and metadiscoursal strategies. Based on the findings, an instructional learning plan is being proposed. This plan is characterized by a genre approach that focuses on expository and linguistic conventions.

Keywords: metadiscourse, organization, theme progression, structure

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Authors: Dong Tang, Yongli Zhao

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The study of the microstructure of asphalt is of great importance for the analysis of its macroscopic properties. However, the peculiarities of the chemical composition of the asphalt itself and the limitations of existing direct imaging techniques have caused researchers to face many obstacles in studying the microstructure of asphalt. The advantage of small-angle X-ray scattering (SAXS) is that it allows quantitative determination of the internal structure of opaque materials and is suitable for analyzing the microstructure of materials. Therefore, the SAXS technique was used to study the evolution of microstructures on the nanoscale during asphalt aging. And the reasons for the change in scattering contrast during asphalt aging were also explained with the help of Fourier transform infrared spectroscopy (FTIR). SAXS experimental results show that the SAXS curves of asphalt are similar to the scattering curves of scattering objects with two-level structures. The Porod curve for asphalt shows that there is no obvious interface between the micelles and the surrounding mediums, and there is only a fluctuation of the hot electron density between the two. The Beaucage model fit SAXS patterns shows that the scattering coefficient P of the asphaltene clusters as well as the size of the micelles, gradually increase with the aging of the asphalt. Furthermore, aggregation exists between the micelles of asphalt and becomes more pronounced with increasing aging. During asphalt aging, the electron density difference between the micelles and the surrounding mediums gradually increases, leading to an increase in the scattering contrast of the asphalt. Under long-term aging conditions due to the gradual transition from maltenes to asphaltenes, the electron density difference between the micelles and the surrounding mediums decreases, resulting in a decrease in the scattering contrast of asphalt SAXS. Finally, this paper correlates the macroscopic properties of asphalt with microstructural parameters, and the results show that the high-temperature rutting resistance of asphalt is enhanced and the low-temperature cracking resistance decreases due to the aggregation of micelles and the generation of new micelles. These results are useful for understanding the relationship between changes in microstructure and changes in properties during asphalt aging and provide theoretical guidance for the regeneration of aged asphalt.

Keywords: asphalt, Beaucage model, microstructure, SAXS

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Authors: Azad Hussain, Andrew Cobley

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The demand for lightweight parts with high mechanical strength(s) and integrity, in sectors such as the aerospace and automotive is ever increasing, motivated by the need for weight reduction in order to increase fuel efficiency with components usually manufactured using a high grade primary metal or alloy. For components manufactured using the squeeze casting process, this alloy is usually A356 aluminium (Al), it is one of the most versatile Al alloys; and is used extensively in castings for demanding environments. The A356 castings provide good strength to weight ratio making it an attractive option for components where strength has to be maintained, with the added advantage of weight reduction. In addition, the versatility in castabilitiy, weldability and corrosion resistance are other attributes that provide for the A356 cast alloy to be used in a large array of industrial applications. Conversely, it is rare to use remelted Al in these cases, due the nature of the applications of components in demanding environments, were material properties must be defined to meet certain specifications for example a known strength or ductility. However the use of remelted Al, especially primary grade Al such as A356, would offer significant cost and energy savings for manufacturers using primary alloys, provided that remelted aluminium can offer similar benefits in terms of material microstructure and mechanical properties. This study presents the results of the material microstructure and properties of 100% primary A356 Al and 100% remelt Al cast, manufactured via the direct squeeze cast method. The microstructures of the castings made from remelted A356 Al were then compared with the microstructures of primary A356 Al. The outcome of using remelting Al on the microstructure was examined via different analytical techniques, optical microscopy of polished and etched surfaces, and scanning electron microscopy. Microstructural analysis of the 100% remelted Al when compared with primary Al show similar α-Al phase, primary Al dendrites, particles and eutectic constituents. Mechanical testing of cast samples will elucidate further information as to the suitability of utilising 100% remelt for casting.

Keywords: A356, microstructure, remelt, squeeze casting

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Authors: M. S. Nandana, K. Udaya Bhat, C. M. Manjunatha

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In this study aluminum alloy 7010 was subjected to three different ageing treatments i.e., peak ageing (T6), over-ageing (T7451) and retrogression and re ageing (RRA) to study the influence of precipitate microstructure on the fatigue crack growth rate behavior. The microstructural modification was studied by using transmission electron microscope (TEM) to examine the change in the size and morphology of precipitates in the matrix and on the grain boundaries. The standard compact tension (CT) specimens were fabricated and tested under constant amplitude fatigue crack growth tests to evaluate the influence of heat treatment on the fatigue crack growth rate properties. The tests were performed in a computer-controlled servo-hydraulic test machine applying a load ratio, R = 0.1 at a loading frequency of 10 Hz as per ASTM E647. The fatigue crack growth was measured by adopting compliance technique using a CMOD gauge attached to the CT specimen. The average size of the matrix precipitates were found to be of 16-20 nm in T7451, 5-6 nm in RRA and 2-3 nm in T6 conditions respectively. The grain boundary precipitate which was continuous in T6, was disintegrated in RRA and T7451 condition. The PFZ width was lower in RRA compared to T7451 condition. The crack growth rate was higher in T7451 and lowest in RRA treated alloy. The RRA treated alloy also exhibits an increase in threshold stress intensity factor range (∆Kₜₕ). The ∆Kₜₕ measured was 11.1, 10.3 and 5.7 MPam¹/² in RRA, T6 and T7451 alloys respectively. The fatigue crack growth rate in RRA treated alloy was nearly 2-3 times lower than that in T6 and was one order lower than that observed in T7451 condition. The surface roughness of RRA treated alloy was more pronounced when compared to the other conditions. The reduction in fatigue crack growth rate in RRA alloy was majorly due to the increase in roughness and partially due to increase in spacing between the matrix precipitates. The reduction in crack growth rate and increase in threshold stress intensity range is expected to benefit the damage tolerant capability of aircraft structural components under service loads.

Keywords: damage tolerance, fatigue, heat treatment, PFZ, RRA

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Authors: Tomasz Łęga, Marta Sosnowska, Mirosława Panasiuk, Lilit Hovhannisyan, Beata Gromadzka, Marcin Olszewski, Sabina Zoledowska, Dawid Nidzworski

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Toxic heavy metal ion contamination of industrial wastewater has recently become a significant environmental concern in many regions of the world. Although the majority of heavy metals are naturally occurring elements found on the earth's surface, anthropogenic activities such as mining and smelting, industrial production, and agricultural use of metals and metal-containing compounds are responsible for the majority of environmental contamination and human exposure. The permissible limits (ppm) for heavy metals in food, water and soil are frequently exceeded and considered hazardous to humans, other organisms, and the environment as a whole. Human exposure to highly nickel-polluted environments causes a variety of pathologic effects. In 2008, nickel received the shameful name of “Allergen of the Year” (GILLETTE 2008). According to the dermatologist, the frequency of nickel allergy is still growing, and it can’t be explained only by fashionable piercing and nickel devices used in medicine (like coronary stents and endoprostheses). Effective remediation methods for removing heavy metal ions from soil and water are becoming increasingly important. Among others, methods such as chemical precipitation, micro- and nanofiltration, membrane separation, conventional coagulation, electrodialysis, ion exchange, reverse and forward osmosis, photocatalysis and polymer or carbon nanocomposite absorbents have all been investigated so far. The importance of environmentally sustainable industrial production processes and the conservation of dwindling natural resources has highlighted the need for affordable, innovative biosorptive materials capable of recovering specific chemical elements from dilute aqueous solutions. The use of combinatorial phage display techniques for selecting and recognizing material-binding peptides with a selective affinity for any target, particularly inorganic materials, has gained considerable interest in the development of advanced bio- or nano-materials. However, due to the limitations of phage display libraries and the biopanning process, the accuracy of molecular recognition for inorganic materials remains a challenge. This study presents the isolation, identification and characterisation of metal binding phage clones that preferentially recover nickel.

Keywords: Heavy metal recovery, cleaning water, phage display, nickel

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Authors: Q. Ni, J. A. Serna, D. Holland, X. Wang

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The objective of this study is to develop Nuclear Magnetic Resonance (NMR) techniques to enhance bone related research applied on normal and disuse (Biglycan knockout) mice bone in vitro by using both low-field and high-field NMR simultaneously. It is known that the total amplitude of T₂ relaxation envelopes, measured by the Carr-Purcell-Meiboom-Gill NMR spin echo train (CPMG), is a representation of the liquid phase inside the pores. Therefore, the NMR CPMG magnetization amplitude can be transferred to the volume of water after calibration with the NMR signal amplitude of the known volume of the selected water. In this study, the distribution of mobile water, porosity that can be determined by using low-field (20 MHz) CPMG relaxation technique, and the pore size distributions can be determined by a computational inversion relaxation method. It is also known that the total proton intensity of magnetization from the NMR free induction decay (FID) signal is due to the water present inside the pores (mobile water), the water that has undergone hydration with the bone (bound water), and the protons in the collagen and mineral matter (solid-like protons). Therefore, the components of total mobile and bound water within bone that can be determined by low-field NMR free induction decay technique. Furthermore, the bound water in solid phase (mineral and organic constituents), especially, the dominated component of calcium hydroxyapatite (Ca₁₀(OH)₂(PO₄)₆) can be determined by using high-field (400 MHz) magic angle spinning (MAS) NMR. With MAS technique reducing NMR spectral linewidth inhomogeneous broadening and susceptibility broadening of liquid-solid mix, in particular, we can conduct further research into the ¹H and ³¹P elements and environments of bone materials to identify the locations of bound water such as OH- group within minerals and bone architecture. We hypothesize that with low-field and high-field magic angle spinning NMR can provide a more complete interpretation of water distribution, particularly, in bound water, and these data are important to access bone quality and predict the mechanical behavior of bone.

Keywords: bone, mice bone, NMR, water in bone

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Authors: Nikhil Kumar, Asish Bandyopadhyay

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Laser welding process is a capable technology for forming the automobile, microelectronics, marine and aerospace parts etc. In the present work, a mathematical and statistical approach is adopted to study the laser welding of AISI 304 stainless steel. A robotic control 500 W pulsed Nd:YAG laser source with 1064 nm wavelength has been used for welding purpose. Butt joints are made. The effects of welding parameters, namely; laser power, scanning speed and pulse width on the seam width and depth of penetration has been investigated using the empirical models developed by response surface methodology (RSM). Weld quality is directly correlated with the weld geometry. Twenty sets of experiments have been conducted as per central composite design (CCD) design matrix. The second order mathematical model has been developed for predicting the desired responses. The results of ANOVA indicate that the laser power has the most significant effect on responses. Microstructural analysis as well as hardness of the selected weld specimens has been carried out to understand the metallurgical and mechanical behaviour of the weld. Average micro-hardness of the weld is observed to be higher than the base metal. Higher hardness of the weld is the resultant of grain refinement and δ-ferrite formation in the weld structure. The result suggests that the lower line energy generally produce fine grain structure and improved mechanical properties than the high line energy. The combined effects of input parameters on responses have been analyzed with the help of developed 3-D response surface and contour plots. Finally, multi-objective optimization has been conducted for producing weld joint with complete penetration, minimum seam width and acceptable welding profile. Confirmatory tests have been conducted at optimum parametric conditions to validate the applied optimization technique.

Keywords: ANOVA, laser welding, modeling and optimization, response surface methodology

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Authors: Paulomi (Polly) Burey, Zoe Lynch

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In STEM education, students often have difficulty linking static images and words from textbooks or online resources, to the underlying mechanisms of the topic of study. This can often dissuade some students from pursuing study in the physical and chemical sciences. A growing movement in current day students demonstrates that the YouTube generation feel they learn best from video or dynamic, interactive learning tools, and will seek these out as alternatives to their textbooks and the classroom learning environment. Chemistry, and in particular visualization of molecular structures in everyday materials, can prove difficult to comprehend without significant interaction with the teacher of the content and concepts, beyond the timeframe of a typical class. This can cause a learning hurdle for distance education students, and so it is necessary to provide strong electronic tools and resources to aid their learning. As one of the electronic resources, an animation design approach to link everyday materials to their underlying chemistry would be beneficial for student learning, with the focus here being on food. These animations were designed and storyboarded with a scaling approach and commence with a focus on the food material itself and its component parts. This is followed by animated transitions to its underlying microstructure and identifying features, and finally showing the molecules responsible for these microstructural features. The animation ends with a reverse transition back through the molecular structure, microstructure, all the way back to the original food material, and also animates some reactions that may occur during food processing to demonstrate the purpose of the underlying chemistry and how it affects the food we eat. Using this cyclical approach of linking students’ existing knowledge of food to help guide them to understanding more complex knowledge, and then reinforcing their learning by linking back to their prior knowledge again, enhances student understanding. Food is also an ideal material system for students to interact with, in a hands-on manner to further reinforce their learning. These animations were launched this year in a 2nd year University Food Chemistry course with improved learning outcomes for the cohort.

Keywords: chemistry, food science, future pedagogy, STEM Education

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Authors: F. Zouai, F. Z. Benabid, S. Bouhelal, D. Benachour

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Nanocomposite polymer / clay are relatively important area of research. These reinforced plastics have attracted considerable attention in scientific and industrial fields because a very small amount of clay can significantly improve the properties of the polymer. The polymeric matrices used in this work are two saturated polyesters ie polyethylene terephthalate (PET) and polyethylene naphthalate (PEN).The success of processing compatible blends, based on poly(ethylene terephthalate) (PET)/ poly(ethylene naphthalene) (PEN)/clay nanocomposites in one step by reactive melt extrusion is described. Untreated clay was first purified and functionalized ‘in situ’ with a compound based on an organic peroxide/ sulfur mixture and (tetramethylthiuram disulfide) as the activator for sulfur. The PET and PEN materials were first separately mixed in the molten state with functionalized clay. The PET/4 wt% clay and PEN/7.5 wt% clay compositions showed total exfoliation. These compositions, denoted nPET and nPEN, respectively, were used to prepare new n(PET/PEN) nanoblends in the same mixing batch. The n(PET/PEN) nanoblends were compared to neat PET/PEN blends. The blends and nanocomposites were characterized using various techniques. Microstructural and nanostructural properties were investigated. Fourier transform infrared spectroscopy (FTIR) results showed that the exfoliation of tetrahedral clay nanolayers is complete and the octahedral structure totally disappears. It was shown that total exfoliation, confirmed by wide angle X-ray scattering (WAXS) measurements, contributes to the enhancement of impact strength and tensile modulus. In addition, WAXS results indicated that all samples are amorphous. The differential scanning calorimetry (DSC) study indicated the occurrence of one glass transition temperature Tg, one crystallization temperature Tc and one melting temperature Tm for every composition. This was evidence that both PET/PEN and nPET/nPEN blends are compatible in the entire range of compositions. In addition, the nPET/nPEN blends showed lower Tc and higher Tm values than the corresponding neat PET/PEN blends. In conclusion, the results obtained indicate that n(PET/PEN) blends are different from the pure ones in nanostructure and physical behavior.

Keywords: blends, exfoliation, DRX, DSC, montmorillonite, nanocomposites, PEN, PET, plastograph, reactive melt-mixing

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

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

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

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Authors: Sayed M. Ahmed, Sawsan S. Darwish, Nagib A. Elmarzugi, Mohammad A. Al-Dosari, Mahmoud A. Adam, Nadia A. Al-Mouallimi

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Historical stone surfaces and architectural heritage may undergo unwanted changes due to the exposure to many physical and chemical deterioration factors, the innovative properties of the nano - materials can have advantageous application in the restoration and conservation of the cultural heritage with relation to the tailoring of new products for protection and consolidation of stone. The current work evaluates the effectiveness of inorganic compatible treatments; based on nanosized particles of silica (SiO2) dispersed in silicon based product, commonly used as a water-repellent/ consolidation for the construction materials affected by different kinds of decay. The nanocomposites obtained by dispersing the silica nanoparticles in polymeric matrices SILRES® BS OH 100 (solventless mixtures of ethyl silicates), in order to obtain a new nanocomposite, with hydrophobic and consolidation properties, to improve the physical and mechanical properties of the stone material. The nanocomposites obtained and pure SILRES® BS OH 100 were applied by brush Experimental stone blocks. The efficacy of the treatments has been evaluated after consolidation and artificial Thermal aging, through capillary water absorption measurements, Ultraviolet-light exposure to evaluate photo-induced and the hydrophobic effects of the treated surface, Scanning electron microscopy (SEM) examination is performed to evaluate penetration depth, re-aggregating effects of the deposited phase and the surface morphology before and after artificialaging. Sterio microscopy investigation is performed to evaluate the resistant to the effects of the erosion, acids and salts. Improving of stone mechanical properties were evaluated by compressive strength tests, colorimetric measurements were used to evaluate the optical appearance. All the results get together with the apparent effect that, silica/polymer nanocomposite is efficient material for the consolidation of artistic and architectural sandstone monuments, completely compatible, enhanced the durability of sandstone toward thermal and UV aging. In addition, the obtained nanocomposite improved the stone mechanical properties and the resistant to the effects of the erosion, acids and salts compared to the samples treated with pure SILRES® BS OH 100 without silica nanoparticles.

Keywords: colorimetric measurements, compressive strength, nanocomposites, porous stone consolidation, silica nanoparticles, sandstone

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Authors: A. M. Khourshid, I. Sabry

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Friction Stir Welding (FSW), a solid state joining technique, is widely being used for joining Al alloys for aerospace, marine automotive and many other applications of commercial importance. FSW were carried out using a vertical milling machine on Al 5083 alloy pipe. These pipe sections are relatively small in diameter, 5mm, and relatively thin walled, 2 mm. In this study, 5083 aluminum alloy pipe were welded as similar alloy joints using (FSW) process in order to investigate mechanical and microstructural properties .rotation speed 1400 r.p.m and weld speed 10,40,70 mm/min. In order to investigate the effect of welding speeds on mechanical properties, metallographic and mechanical tests were carried out on the welded areas. Vickers hardness profile and tensile tests of the joints as a metallurgical feasibility of friction stir welding for joining Al 6061 aluminum alloy welding was performed on pipe with different thickness 2, 3 and 4 mm,five rotational speeds (485,710,910,1120 and 1400) rpm and a traverse speed (4, 8 and 10)mm/min was applied. This work focuses on two methods such as artificial neural networks using software (pythia) and response surface methodology (RSM) to predict the tensile strength, the percentage of elongation and hardness of friction stir welded 6061 aluminum alloy. An artificial neural network (ANN) model was developed for the analysis of the friction stir welding parameters of 6061 pipe. The tensile strength, the percentage of elongation and hardness of weld joints were predicted by taking the parameters Tool rotation speed, material thickness and travel speed as a function. A comparison was made between measured and predicted data. Response surface methodology (RSM) also developed and the values obtained for the response Tensile strengths, the percentage of elongation and hardness are compared with measured values. The effect of FSW process parameter on mechanical properties of 6061 aluminum alloy has been analyzed in detail.

Keywords: friction stir welding (FSW), al alloys, mechanical properties, microstructure

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Authors: S. Belakry, D. Fasquelle, A. Rolle, E. Capoen, R. N. Vannier, J. C. Carru

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Solid oxide fuel cells (SOFCs) are promising devices for energy conversion due to their high electrical efficiency and eco-friendly behavior. Their performance is not only influenced by the microstructural and electrical properties of the electrodes and electrolyte but also depends on the interactions at the interfaces. Nowadays, commercial SOFCs are electrically efficient at high operating temperatures, typically between 800 and 1000 °C, which restricts their real-life applications. The present work deals with the objectives to reduce the operating temperature and to develop cost-effective intermediate-temperature solid oxide fuel cells (IT-SOFCs). This work focuses on the development of metal-supported solid oxide fuel cells (MS-IT-SOFCs) that would provide cheaper SOFC cells with increased lifetime and reduced operating temperature. In the framework, the local company TIBTECH brings its skills for the manufacturing of porous metal supports. This part of the work focuses on the physical, chemical, and electrical characterizations of porous metallic supports (stainless steel 316 L and FeCrAl alloy) under different exposure conditions of temperature and atmosphere by studying oxidation, mechanical resistance, and electrical conductivity of the materials. Within the target operating temperature (i.e., 500 to 700 ° C), the stainless steel 316 L and FeCrAl alloy slightly oxidize in the air and H2, but don’t deform; whereas under Ar atmosphere, they oxidize more than with previously mentioned atmospheres. Above 700 °C under air and Ar, the two metallic supports undergo high oxidation. From 500 to 700 °C, the resistivity of FeCrAl increases by 55%. But nevertheless, the FeCrAl resistivity increases more slowly than the stainless steel 316L resistivity. This study allows us to verify the compatibility of electrodes and electrolyte materials with metallic support at the operating requirements of the IT-SOFC cell. The characterizations made in this context will also allow us to choose the most suitable fabrication process for all functional layers in order to limit the oxidation of the metallic supports.

Keywords: stainless steel 316L, FeCrAl alloy, solid oxide fuel cells, porous metallic support

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Authors: L. Vivet, L. Benabou, O. Simon

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With highly demanding applications in the field of power electronics, there is an increasing need to have interconnection materials with properties that can ensure both good mechanical assembly and high thermal/electrical conductivities. So far, lead-free solders have been considered an attractive solution, but recently, sintered joints based on nano-silver paste have been used for die attach and have proved to be a promising solution offering increased performances in high-temperature applications. In this work, the main parameters of the bonding process using silver oxalates are studied, i.e., the heating rate and the bonding pressure mainly. Their effects on both the mechanical and thermal properties of the sintered layer are evaluated following an experimental design. Pairs of copper substrates with gold metallization are assembled through the sintering process to realize the samples that are tested using a micro-traction machine. In addition, the obtained joints are examined through microscopy to identify the important microstructural features in relation to the measured properties. The formation of an intermetallic compound at the junction between the sintered silver layer and the gold metallization deposited on copper is also analyzed. Microscopy analysis exhibits a nanoporous structure of the sintered material. It is found that higher temperature and bonding pressure result in higher densification of the sintered material, with higher thermal conductivity of the joint but less mechanical flexibility to accommodate the thermo-mechanical stresses arising during service. The experimental design allows hence the determination of the optimal process parameters to reach sufficient thermal/mechanical properties for a given application. It is also found that the interphase formed between silver and gold metallization is the location where the fracture occurred after the mechanical testing, suggesting that the inter-diffusion mechanism between the different elements of the assembly leads to the formation of a relatively brittle compound.

Keywords: nanoporous structure, silver oxalate, sintering, mechanical strength, thermal conductivity, microelectronic packaging

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Authors: Igor Jerkovic

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Biodiversity of flora provides many different nectar sources for the bees. Unifloral honeys possess distinctive flavours, mainly derived from their nectar sources (characteristic volatile organic components (VOCs)). Specific or nonspecific VOCs (chemical markers) could be used for unifloral honey characterisation as addition to the melissopalynologycal analysis. The main honey volatiles belong, in general, to three principal categories: terpenes, norisoprenoids, and benzene derivatives. Some of these substances have been described as characteristics of the floral source, and other compounds, like several alcohols, branched aldehydes, and furan derivatives, may be related to the microbial purity of honey processing and storage conditions. Selection of the extraction method for the honey volatiles profiling should consider that heating of the honey produce different artefacts and therefore conventional methods of VOCs isolation (such as hydrodistillation) cannot be applied for the honey. Two-way approach for the isolation of the honey VOCs was applied using headspace solid-phase microextraction (HS-SPME) and ultrasonic solvent extraction (USE). The extracts were analysed by gas chromatography and mass spectrometry (GC-MS). HS-SPME (with the fibers of different polarity such as polydimethylsiloxane/ divinylbenzene (PDMS/DVB) or divinylbenzene/carboxene/ polydimethylsiloxane (DVB/CAR/PDMS)) enabled isolation of high volatile headspace VOCs of the honey samples. Among them, some characteristic or specific compounds can be found such as 3,4-dihydro-3-oxoedulan (in Centaurea cyanus L. honey) or 1H-indole, methyl anthranilate, and cis-jasmone (in Citrus unshiu Marc. honey). USE with different solvents (mainly dichloromethane or the mixture pentane : diethyl ether 1 : 2 v/v) enabled isolation of less volatile and semi-volatile VOCs of the honey samples. Characteristic compounds from C. unshiu honey extracts were caffeine, 1H-indole, 1,3-dihydro-2H-indol-2-one, methyl anthranilate, and phenylacetonitrile. Sometimes, the selection of solvent sequence was useful for more complete profiling such as sequence I: pentane → diethyl ether or sequence II: pentane → pentane/diethyl ether (1:2, v/v) → dichloromethane). The extracts with diethyl ether contained hydroquinone and 4-hydroxybenzoic acid as the major compounds, while (E)-4-(r-1’,t-2’,c-4’-trihydroxy-2’,6’,6’-trimethylcyclo-hexyl)but-3-en-2-one predominated in dichloromethane extracts of Allium ursinum L. honey. With this two-way approach, it was possible to obtain a more detailed insight into the honey volatile and semi-volatile compounds and to minimize the risks of compound discrimination due to their partial extraction that is of significant importance for the complete honey profiling and identification of the chemical biomarkers that can complement the pollen analysis.

Keywords: honey chemical biomarkers, honey volatile compounds profiling, headspace solid-phase microextraction (HS-SPME), ultrasonic solvent extraction (USE)

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Authors: Rajeev Ravindran, Amit K. Jaiswal

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Lignocellulose is the largest reservoir of inexpensive, renewable source of carbon. It is composed of lignin, cellulose and hemicellulose. Cellulose and hemicellulose is composed of reducing sugars glucose, xylose and several other monosaccharides which can be metabolised by microorganisms to produce several value added products such as biofuels, enzymes, aminoacids etc. Enzymatic treatment of lignocellulose leads to the release of monosaccharides such as glucose and xylose. However, factors such as the presence of lignin, crystalline cellulose, acetyl groups, pectin etc. contributes to recalcitrance restricting the effective enzymatic hydrolysis of cellulose and hemicellulose. In order to overcome these problems, pre-treatment of lignocellulose is generally carried out which essentially facilitate better degradation of lignocellulose. A range of pre-treatment strategy is commonly employed based on its mode of action viz. physical, chemical, biological and physico-chemical. However, existing pretreatment strategies result in lower sugar yield and formation of inhibitory compounds. In order to overcome these problems, we proposes a novel pre-treatment, which utilises the superior oxidising capacity of alkaline potassium permanganate assisted by ultra-sonication to break the covalent bonds in spent coffee waste to remove recalcitrant compounds such as lignin. The pre-treatment was conducted for 30 minutes using 2% (w/v) potassium permanganate at room temperature with solid to liquid ratio of 1:10. The pre-treated spent coffee waste (SCW) was subjected to enzymatic hydrolysis using enzymes cellulase and hemicellulase. Shake flask experiments were conducted with a working volume of 50mL buffer containing 1% substrate. The results showed that the novel pre-treatment strategy yielded 7 g/L of reducing sugar as compared to 3.71 g/L obtained from biomass that had undergone dilute acid hydrolysis after 24 hours. From the results obtained it is fairly certain that ultrasonication assists the oxidation of recalcitrant components in lignocellulose by potassium permanganate. Enzyme hydrolysis studies suggest that ultrasound assisted alkaline potassium permanganate pre-treatment is far superior over treatment by dilute acid. Furthermore, SEM, XRD and FTIR were carried out to analyse the effect of the new pre-treatment strategy on structure and crystallinity of pre-treated spent coffee wastes. This novel one-step pre-treatment strategy was implemented under mild conditions and exhibited high efficiency in the enzymatic hydrolysis of spent coffee waste. Further study and scale up is in progress in order to realise future industrial applications.

Keywords: spent coffee waste, alkaline potassium permanganate, ultra-sonication, physical characterisation

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Authors: T. Ferreira, A. Kulkarni, C. Bretscher, K. Richter, M. Ehrlich, A. Marchini

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H-1 protoparvovirus (H-1PV) is a virus with inherent oncolytic and oncosuppressive activities while remaining non-pathogenic in humans. H-1PV was the first oncolytic parvovirus to undergo clinical testing. Results from trials in patients with glioblastoma or pancreatic carcinoma showed an excellent safety profile and first signs of efficacy. H-1PV infection is vastly dependent on cellular factors, from cell attachment and entry to viral replication and egress. Hence, we believe that the characterisation of the parvovirus life cycle would ultimately help further improve H-1PV clinical outcome. In the present study, we explored the entry pathway of H-1PV in cervical HeLa and glioma NCH125 cancer cell lines. Electron and confocal microscopy showed viral particles associated with clathrin-coated pits and vesicles, providing the first evidence that H-1PV cell entry occurs through clathrin-mediated endocytosis. Accordingly, we observed that by blocking clathrin-mediated endocytosis with hypertonic sucrose, chlorpromazine, or pitstop 2, H-1PV transduction was markedly decreased. Accordingly, siRNA-mediated knockdown of AP2M1, which retains a crucial role in clathrin-mediated endocytosis, verified the reliance of H-1PV on this route to enter HeLa and NCH125 cancer cells. By contrast, we found no evidence of viral entry through caveolae-mediated endocytosis. Indeed, pre-treatment of cells with nystatin or methyl-β-cyclodextrin, both inhibitors of caveolae-mediated endocytosis, did not affect viral transduction levels. Unexpectedly, siRNA-mediated knockdown of caveolin-1, the main driver of caveolae-mediated endocytosis, increased H-1PV transduction, suggesting caveolin-1 is a negative modulator of H-1PV infection. We also show that H-1PV entry is dependent on dynamin, a protein responsible for mediating the scission of vesicle neck and promoting further internalisation. Furthermore, since dynamin inhibition almost completely abolished H-1PV infection, makes it unlikely that H-1PV uses macropinocytosis as an alternative pathway to enter cells. After viral internalisation, H-1PV passes through early to late endosomes as observed by confocal microscopy. Inside these endocytic compartments, the acidic environment proved to be crucial for a productive infection. Inhibition of acidification of pH dramatically reduced H-1PV transduction. Besides, a fraction of H-1PV particles was observed inside LAMP1-positive lysosomes, most likely following a non-infectious route. To the author's best knowledge, this is the first study to characterise the cell entry pathways of H-1PV. Along these lines, this work will further contribute to understand H-1PV oncolytic properties as well as to improve its clinical potential in cancer virotherapy.

Keywords: clathrin-mediated endocytosis, H-1 parvovirus, oncolytic virus, virus entry

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