Search results for: metastable titanium alloy
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 1089

Search results for: metastable titanium alloy

69 Electron Beam Melting Process Parameter Optimization Using Multi Objective Reinforcement Learning

Authors: Michael A. Sprayberry, Vincent C. Paquit

Abstract:

Process parameter optimization in metal powder bed electron beam melting (MPBEBM) is crucial to ensure the technology's repeatability, control, and industry-continued adoption. Despite continued efforts to address the challenges via the traditional design of experiments and process mapping techniques, there needs to be more successful in an on-the-fly optimization framework that can be adapted to MPBEBM systems. Additionally, data-intensive physics-based modeling and simulation methods are difficult to support by a metal AM alloy or system due to cost restrictions. To mitigate the challenge of resource-intensive experiments and models, this paper introduces a Multi-Objective Reinforcement Learning (MORL) methodology defined as an optimization problem for MPBEBM. An off-policy MORL framework based on policy gradient is proposed to discover optimal sets of beam power (P) – beam velocity (v) combinations to maintain a steady-state melt pool depth and phase transformation. For this, an experimentally validated Eagar-Tsai melt pool model is used to simulate the MPBEBM environment, where the beam acts as the agent across the P – v space to maximize returns for the uncertain powder bed environment producing a melt pool and phase transformation closer to the optimum. The culmination of the training process yields a set of process parameters {power, speed, hatch spacing, layer depth, and preheat} where the state (P,v) with the highest returns corresponds to a refined process parameter mapping. The resultant objects and mapping of returns to the P-v space show convergence with experimental observations. The framework, therefore, provides a model-free multi-objective approach to discovery without the need for trial-and-error experiments.

Keywords: additive manufacturing, metal powder bed fusion, reinforcement learning, process parameter optimization

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68 Thorium-Doped PbS Thin Films for Radiation Damage Studies

Authors: Michael Shandalov, Tzvi Templeman, Michael Schmidt, Itzhak Kelson, Eyal Yahel

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We present a new method to produce a model system for the study of radiation damage in non-radioactive materials. The method is based on homogeneously incorporating 228Th ions in PbS thin films using a small volume chemical bath deposition (CBD) technique. The common way to alloy metals with radioactive elements is by melting pure elements, which requires considerable amounts of radioactive material with its safety consequences such as high sample activity. Controlled doping of the thin films with (very) small amounts (100-200ppm) of radioactive elements such as thorium is expected to provide a unique path for studying radiation damage in materials due to decay processes without the need of sealed enclosure. As a first stage, we developed CBD process for controlled doping of PbS thin films (~100 nm thick) with the stable isotope (t1/2~106 years), 232Th. Next, we developed CBD process for controlled doping of PbS thin films with active 228Th isotope. This was achieved by altering deposition parameters such as temperature, pH, reagent concentrations and time. The 228Th-doped films were characterized using X-ray diffraction, which indicated a single phase material. Film morphology and thickness were determined using scanning electron microscopy (SEM). Energy dispersive spectroscopy (EDS) mapping in the analytical transmission electron microscope (A-TEM), X-ray photoelectron spectroscopy (XPS) depth profiles and autoradiography indicated that the Th ions were homogeneously distributed throughout the films, suggesting Pb substitution by Th ions in the crystal lattice. The properties of the PbS (228Th) film activity were investigated by using alpha-spectroscopy and gamma spectroscopy. The resulting films are applicable for isochronal annealing of resistivity measurements and currently under investigation. This work shows promise as a model system for the analysis of dilute defect systems in semiconductor thin films.

Keywords: thin films, doping, radiation damage, chemical bath deposition

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67 A Low-Cost Memristor Based on Hybrid Structures of Metal-Oxide Quantum Dots and Thin Films

Authors: Amir Shariffar, Haider Salman, Tanveer Siddique, Omar Manasreh

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According to the recent studies on metal-oxide memristors, researchers tend to improve the stability, endurance, and uniformity of resistive switching (RS) behavior in memristors. Specifically, the main challenge is to prevent abrupt ruptures in the memristor’s filament during the RS process. To address this problem, we are proposing a low-cost hybrid structure of metal oxide quantum dots (QDs) and thin films to control the formation of filaments in memristors. We aim to use metal oxide quantum dots because of their unique electronic properties and quantum confinement, which may improve the resistive switching behavior. QDs have discrete energy spectra due to electron confinement in three-dimensional space. Because of Coulomb repulsion between electrons, only a few free electrons are contained in a quantum dot. This fact might guide the growth direction for the conducting filaments in the metal oxide memristor. As a result, it is expected that QDs can improve the endurance and uniformity of RS behavior in memristors. Moreover, we use a hybrid structure of intrinsic n-type quantum dots and p-type thin films to introduce a potential barrier at the junction that can smooth the transition between high and low resistance states. A bottom-up approach is used for fabricating the proposed memristor using different types of metal-oxide QDs and thin films. We synthesize QDs including, zinc oxide, molybdenum trioxide, and nickel oxide combined with spin-coated thin films of titanium dioxide, copper oxide, and hafnium dioxide. We employ fluorine-doped tin oxide (FTO) coated glass as the substrate for deposition and bottom electrode. Then, the active layer composed of one type of quantum dots, and the opposite type of thin films is spin-coated onto the FTO. Lastly, circular gold electrodes are deposited with a shadow mask by using electron-beam (e-beam) evaporation at room temperature. The fabricated devices are characterized using a probe station with a semiconductor parameter analyzer. The current-voltage (I-V) characterization is analyzed for each device to determine the conduction mechanism. We evaluate the memristor’s performance in terms of stability, endurance, and retention time to identify the optimal memristive structure. Finally, we assess the proposed hypothesis before we proceed to the optimization process for fabricating the memristor.

Keywords: memristor, quantum dot, resistive switching, thin film

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66 Enhancing Photocatalytic Hydrogen Production: Modification of TiO₂ by Coupling with Semiconductor Nanoparticles

Authors: Saud Hamdan Alshammari

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Photocatalytic water splitting to produce hydrogen (H₂) has obtained significant attention as an environmentally friendly technology. This process, which produces hydrogen from water and sunlight, represents a renewable energy source. Titanium dioxide (TiO₂) plays a critical role in photocatalytic hydrogen production due to its chemical stability, availability, and low cost. Nevertheless, TiO₂'s wide band gap (3.2 eV) limits its visible light absorption and might affect the effectiveness of the photocatalytic. Coupling TiO₂ with other semiconductors is a strategy that can enhance TiO₂ by narrowing its band gap and improving visible light absorption. This paper studies the modification of TiO₂ by coupling it with another semiconductor such as CdS nanoparticles using a reflux reactor and autoclave reactor that helps form a core-shell structure. Characterization techniques, including TEM and UV-Vis spectroscopy, confirmed successful coating of TiO₂ on CdS core, reduction of the band gap from 3.28 eV to 3.1 eV, and enhanced light absorption in the visible region. These modifications are attributed to the heterojunction structure between TiO₂ and CdS.The essential goal of this study is to improve TiO₂ for use in photocatalytic water splitting to enhance hydrogen production. The core-shell TiO₂@CdS nanoparticles exhibited promising results, due to band gap narrowing and improved light absorption. Future work will involve adding Pt as a co-catalyst, which is known to increase surface reaction activity by enhancing proton adsorption. Evaluation of the TiO₂@CdS@Pt catalyst will include performance assessments and hydrogen productivity tests, considering factors such as effective shapes and material ratios. Moreover, the study could be enhanced by studying further modifications to the catalyst and displaying additional performance evaluations. For instance, doping TiO₂ with metals such as nickel (Ni), iron (Fe), and cobalt (Co) and non-metals such as nitrogen (N), carbon (C), and sulfur (S) could positively influence the catalyst by reducing the band gap, enhancing the separation of photogenerated electron-hole pairs, and increasing the surface area, respectively. Additionally, to further improve catalytic performance, examining different catalyst morphologies, such as nanorods, nanowires, and nanosheets, in hydrogen production could be highly beneficial. Optimizing photoreactor design for efficient photon delivery and illumination will further enhance the photocatalytic process. These strategies collectively aim to overcome current challenges and improve the efficiency of hydrogen production via photocatalysis.

Keywords: hydrogen production, photocatalytic, water spliiting, semiconductor, nanoparticles

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65 Effects of Machining Parameters on the Surface Roughness and Vibration of the Milling Tool

Authors: Yung C. Lin, Kung D. Wu, Wei C. Shih, Jui P. Hung

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High speed and high precision machining have become the most important technology in manufacturing industry. The surface roughness of high precision components is regarded as the important characteristics of the product quality. However, machining chatter could damage the machined surface and restricts the process efficiency. Therefore, selection of the appropriate cutting conditions is of importance to prevent the occurrence of chatter. In addition, vibration of the spindle tool also affects the surface quality, which implies the surface precision can be controlled by monitoring the vibration of the spindle tool. Based on this concept, this study was aimed to investigate the influence of the machining conditions on the surface roughness and the vibration of the spindle tool. To this end, a series of machining tests were conducted on aluminum alloy. In tests, the vibration of the spindle tool was measured by using the acceleration sensors. The surface roughness of the machined parts was examined using white light interferometer. The response surface methodology (RSM) was employed to establish the mathematical models for predicting surface finish and tool vibration, respectively. The correlation between the surface roughness and spindle tool vibration was also analyzed by ANOVA analysis. According to the machining tests, machined surface with or without chattering was marked on the lobes diagram as the verification of the machining conditions. Using multivariable regression analysis, the mathematical models for predicting the surface roughness and tool vibrations were developed based on the machining parameters, cutting depth (a), feed rate (f) and spindle speed (s). The predicted roughness is shown to agree well with the measured roughness, an average percentage of errors of 10%. The average percentage of errors of the tool vibrations between the measurements and the predictions of mathematical model is about 7.39%. In addition, the tool vibration under various machining conditions has been found to have a positive influence on the surface roughness (r=0.78). As a conclusion from current results, the mathematical models were successfully developed for the predictions of the surface roughness and vibration level of the spindle tool under different cutting condition, which can help to select appropriate cutting parameters and to monitor the machining conditions to achieve high surface quality in milling operation.

Keywords: machining parameters, machining stability, regression analysis, surface roughness

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64 Experimental Investigation of the Thermal Conductivity of Neodymium and Samarium Melts by a Laser Flash Technique

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

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63 Cu₂(ZnSn)(S)₄ Electrodeposition from a Single Bath for Photovoltaic Applications

Authors: Mahfouz Saeed

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Cu₂(ZnSn)(S)₄ (CTZS) offers potential advantages over CuInGaSe₂ (CIGS) as solar thin film because to its higher band gap. Preparing such photovoltaic materials by electrochemical techniques is particularly attractive due to the lower processing cost and the high throughput of such techniques. Several recent publications report CTZS electroplating; however, the electrochemical process still facing serious challenges such as a sulfur atomic ration which is about 50% of the total alloy. We introduce in this work an improved electrolyte composition which enables the direct electrodeposition of CTZS from a single bath. The electrolyte is significantly more dilute in comparison to common baths described in the literature. The bath composition we introduce is: 0.0032 M CuSO₄, 0.0021 M ZnSO₄, 0.0303 M SnCl₂, 0.0038 M Na₂S₂O₃, and 0.3 mM Na₂S₂O3. PHydrion is applied to buffer the electrolyte to pH=2, and 0.7 M LiCl is applied as supporting electrolyte. Electrochemical process was carried at a rotating disk electrode which provides quantitative characterization of the flow (room temperature). Comprehensive electrochemical behavior study at different electrode rotation rates are provided. The effects of agitation on atomic composition of the deposit and its adhesion to the molybdenum back contact are discussed. The post treatment annealing was conducted under sulfur atmosphere with no need for metals addition from the gas phase during annealing. The potential which produced the desired atomic ratio of CTZS at -0.82 V/NHE. Smooth deposit, with uniform composition across the sample surface and depth was obtained at 500 rpm rotation speed. Final sulfur atomic ratio was adjusted to 50.2% in order to have the desired atomic ration. The final composition was investigated using Energy-dispersive X-ray spectroscopy technique (EDS). XRD technique used to analyze CTZS crystallography and thickness. Complete and functional CTZS PV devices were fabricated by depositing all the required layers in the correct order and the desired optical properties. Acknowledgments: Case Western Reserve University for the technical help and for using their instruments.

Keywords: photovoltaic, CTZS, thin film, electrochemical

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62 Effect of Self-Lubricating Carbon Materials on the Tribological Performance of Ultra-High Molecular Weight Polyethylene

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

Abstract:

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

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

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61 Finite Element Analysis of Mechanical Properties of Additively Manufactured 17-4 PH Stainless Steel

Authors: Bijit Kalita, R. Jayaganthan

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Additive manufacturing (AM) is a novel manufacturing method which provides more freedom in design, manufacturing near-net-shaped parts as per demand, lower cost of production, and expedition in delivery time to market. Among various metals, AM techniques, Laser Powder Bed Fusion (L-PBF) is the most prominent one that provides higher accuracy and powder proficiency in comparison to other methods. Particularly, 17-4 PH alloy is martensitic precipitation hardened (PH) stainless steel characterized by resistance to corrosion up to 300°C and tailorable strengthening by copper precipitates. Additively manufactured 17-4 PH stainless steel exhibited a dendritic/cellular solidification microstructure in the as-built condition. It is widely used as a structural material in marine environments, power plants, aerospace, and chemical industries. The excellent weldability of 17-4 PH stainless steel and its ability to be heat treated to improve mechanical properties make it a good material choice for L-PBF. In this study, the microstructures of martensitic stainless steels in the as-built state, as well as the effects of process parameters, building atmosphere, and heat treatments on the microstructures, are reviewed. Mechanical properties of fabricated parts are studied through micro-hardness and tensile tests. Tensile tests are carried out under different strain rates at room temperature. In addition, the effect of process parameters and heat treatment conditions on mechanical properties is critically reviewed. These studies revealed the performance of L-PBF fabricated 17–4 PH stainless-steel parts under cyclic loading, and the results indicated that fatigue properties were more sensitive to the defects generated by L-PBF (e.g., porosity, microcracks), leading to the low fracture strains and stresses under cyclic loading. Rapid melting, solidification, and re-melting of powders during the process and different combinations of processing parameters result in a complex thermal history and heterogeneous microstructure and are necessary to better control the microstructures and properties of L-PBF PH stainless steels through high-efficiency and low-cost heat treatments.

Keywords: 17–4 PH stainless steel, laser powder bed fusion, selective laser melting, microstructure, additive manufacturing

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60 Synthesized Doped TiO2 Photocatalysts for Mineralization of Quinalphos from Aqueous Streams

Authors: Nidhi Sharotri, Dhiraj Sud

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Water pollution by pesticides constitutes a serious ecological problem due to their potential toxicity and bioaccumulation. The widespread use of pesticides in industry and agriculture along with their resistance to natural decomposition, biodegradation, chemical and photochemical degradation under typical environmental conditions has resulted in the emergence of these chemicals and their transformed products in natural water. Among AOP’s, heterogeneous photocatalysis using TiO2 as photocatalyst appears as the most emerging destructive technology for mineralization of the pollutant in aquatic streams. Among the various semiconductors (TiO2, ZnO, CdS, FeTiO3, MnTiO3, SrTiO2 and SnO2), TiO2 has proven to be the most efficient photocatalyst for environmental applications due to its biological and chemical inertness, high photo reactivity, non-toxicity, and photo stability. Semiconductor photocatalysts are characterized by an electronic band structure in which valence band and conduction band are separated by a band gap, i.e. a region of forbidden energy. Semiconductor based photocatalysts produces e-/h+ pairs which have been employed for degradation of organic pollutants. The present paper focuses on modification of TiO2 photocatalyst in order to shift its absorption edge towards longer wavelength to make it active under natural light. Semiconductor TiO2 photocatalysts was prepared by doping with anion (N), cation (Mn) and double doped (Mn, N) using greener approach. Titanium isopropoxide is used as titania precursor and ethanedithiol, hydroxyl amine hydrochloride, manganous chloride as sulphur, nitrogen and manganese precursors respectively. Synthesized doped TiO2 nanomaterials are characterized for surface morphology (SEM, TEM), crystallinity (XRD) and optical properties (absorption spectra and band gap). EPR data confirms the substitutional incorporation of Mn2+ in TiO2 lattice. The doping influences the phase transformation of rutile and anatase phase crystal and thereby the absorption spectrum changes were observed. The effect of variation of reaction parameters such as solvent, reaction time and calcination temperature on the yield, surface morphology and optical properties was also investigated. The TEM studies show the particle size of nanomaterials varies from 10-50 nm. The calculated band gap of nanomaterials varies from 2.30-2.60 eV. The photocatalytic degradation of organic pollutant organophosphate pesticide (Quinalphos) has been investigated by studying the changes in UV absorption spectrum and the promising results were obtained under visible light. The complete mineralization of quinalphos has occurred as no intermediates were recorded after 8 hrs of degradation confirmed from the HPLC studies.

Keywords: quinalphos, doped-TiO2, mineralization, EPR

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59 Effect of Varying Zener-Hollomon Parameter (Temperature and Flow Stress) and Stress Relaxation on Creep Response of Hot Deformed AA3104 Can Body Stock

Authors: Oyindamola Kayode, Sarah George, Roberto Borrageiro, Mike Shirran

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A phenomenon identified by our industrial partner has experienced sag on AA3104 can body stock (CBS) transfer bar during transportation of the slab from the breakdown mill to the finishing mill. Excessive sag results in bottom scuffing of the slab onto the roller table, resulting in surface defects on the final product. It has been found that increasing the strain rate on the breakdown mill final pass results in a slab resistant to sag. The creep response for materials hot deformed at different Zener–Holloman parameter values needs to be evaluated experimentally to gain better understanding of the operating mechanism. This study investigates this identified phenomenon through laboratory simulation of the breakdown mill conditions for various strain rates by utilizing the Gleeble at UCT Centre for Materials Engineering. The experiment will determine the creep response for a range of conditions as well as quantifying the associated material microstructure (sub-grain size, grain structure etc). The experimental matrices were determined based on experimental conditions approximate to industrial hot breakdown rolling and carried out on the Gleeble 3800 at the Centre for Materials Engineering, University of Cape Town. Plane strain compression samples were used for this series of tests at an applied load that allow for better contact and exaggerated creep displacement. A tantalum barrier layer was used for increased conductivity and decreased risk of anvil welding. One set of tests with no in-situ hold time was performed, where the samples were quenched after deformation. The samples were retained for microstructure analysis of the micrographs from the light microscopy (LM), quantitative data and images from scanning electron microscopy (SEM) and energy dispersive X-ray (EDX), sub-grain size and grain structure from electron back scattered diffraction (EBSD).

Keywords: aluminium alloy, can-body stock, hot rolling, creep response, Zener-Hollomon parameter

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58 Customized Temperature Sensors for Sustainable Home Appliances

Authors: Merve Yünlü, Nihat Kandemir, Aylin Ersoy

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Temperature sensors are used in home appliances not only to monitor the basic functions of the machine but also to minimize energy consumption and ensure safe operation. In parallel with the development of smart home applications and IoT algorithms, these sensors produce important data such as the frequency of use of the machine, user preferences, and the compilation of critical data in terms of diagnostic processes for fault detection throughout an appliance's operational lifespan. Commercially available thin-film resistive temperature sensors have a well-established manufacturing procedure that allows them to operate over a wide temperature range. However, these sensors are over-designed for white goods applications. The operating temperature range of these sensors is between -70°C and 850°C, while the temperature range requirement in home appliance applications is between 23°C and 500°C. To ensure the operation of commercial sensors in this wide temperature range, usually, a platinum coating of approximately 1-micron thickness is applied to the wafer. However, the use of platinum in coating and the high coating thickness extends the sensor production process time and therefore increases sensor costs. In this study, an attempt was made to develop a low-cost temperature sensor design and production method that meets the technical requirements of white goods applications. For this purpose, a custom design was made, and design parameters (length, width, trim points, and thin film deposition thickness) were optimized by using statistical methods to achieve the desired resistivity value. To develop thin film resistive temperature sensors, one side polished sapphire wafer was used. To enhance adhesion and insulation 100 nm silicon dioxide was coated by inductively coupled plasma chemical vapor deposition technique. The lithography process was performed by a direct laser writer. The lift-off process was performed after the e-beam evaporation of 10 nm titanium and 280 nm platinum layers. Standard four-point probe sheet resistance measurements were done at room temperature. The annealing process was performed. Resistivity measurements were done with a probe station before and after annealing at 600°C by using a rapid thermal processing machine. Temperature dependence between 25-300 °C was also tested. As a result of this study, a temperature sensor has been developed that has a lower coating thickness than commercial sensors but can produce reliable data in the white goods application temperature range. A relatively simplified but optimized production method has also been developed to produce this sensor.

Keywords: thin film resistive sensor, temperature sensor, household appliance, sustainability, energy efficiency

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57 Effect of Ramp Rate on the Preparation of Activated Carbon from Saudi Date Tree Fronds (Agro Waste) by Physical Activation Method

Authors: Muhammad Shoaib, Hassan M Al-Swaidan

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Saudi Arabia is the major date producer in the world. In order to maximize the production from date tree, pruning of the date trees is required annually. Large amount of this agriculture waste material (palm tree fronds) is available in Saudi Arabia and considered as an ideal source as a precursor for production of activated carbon (AC). The single step procedure for the preparation of micro porous activated carbon (AC) from Saudi date tree fronds using mixture of gases (N2 and CO2) is carried out at carbonization/activation temperature at 850°C and at different ramp rates of 10, 20 and 30 degree per minute. Alloy 330 horizontal reactor is used for tube furnace. Flow rate of nitrogen and carbon dioxide gases are kept at 150 ml/min and 50 ml/min respectively during the preparation. Characterization results reveal that the BET surface area, pore volume, and average pore diameter of the resulting activated carbon generally decreases with the increase in ramp rate. The activated carbon prepared at a ramp rate of 10 degrees/minute attains larger surface area and can offer higher potential to produce activated carbon of greater adsorption capacity from agriculture wastes such as date fronds. The BET surface areas of the activated carbons prepared at a ramp rate of 10, 20 and 30 degree/minute after 30 minutes activation time are 1094, 1020 and 515 m2/g, respectively. Scanning electron microscopy (SEM) for surface morphology, and FTIR for functional groups was carried out that also verified the same trend. Moreover, by increasing the ramp rate from 10 and 20 degrees/min the yield remains same, i.e. 18%, whereas at a ramp rate of 30 degrees/min the yield increases from 18 to 20%. Thus, it is feasible to produce high-quality micro porous activated carbon from date frond agro waste using N2 carbonization followed by physical activation with CO2 and N2 mixture. This micro porous activated carbon can be used as adsorbent of heavy metals from wastewater, NOx SOx emission adsorption from ambient air and electricity generation plants, purification of gases, sewage treatment and many other applications.

Keywords: activated carbon, date tree fronds, agricultural waste, applied chemistry

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56 Preliminary Evaluation of Decommissioning Wastes for the First Commercial Nuclear Power Reactor in South Korea

Authors: Kyomin Lee, Joohee Kim, Sangho Kang

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The commercial nuclear power reactor in South Korea, Kori Unit 1, which was a 587 MWe pressurized water reactor that started operation since 1978, was permanently shut down in June 2017 without an additional operating license extension. The Kori 1 Unit is scheduled to become the nuclear power unit to enter the decommissioning phase. In this study, the preliminary evaluation of the decommissioning wastes for the Kori Unit 1 was performed based on the following series of process: firstly, the plant inventory is investigated based on various documents (i.e., equipment/ component list, construction records, general arrangement drawings). Secondly, the radiological conditions of systems, structures and components (SSCs) are established to estimate the amount of radioactive waste by waste classification. Third, the waste management strategies for Kori Unit 1 including waste packaging are established. Forth, selection of the proper decontamination and dismantling (D&D) technologies is made considering the various factors. Finally, the amount of decommissioning waste by classification for Kori 1 is estimated using the DeCAT program, which was developed by KEPCO-E&C for a decommissioning cost estimation. The preliminary evaluation results have shown that the expected amounts of decommissioning wastes were less than about 2% and 8% of the total wastes generated (i.e., sum of clean wastes and radwastes) before/after waste processing, respectively, and it was found that the majority of contaminated material was carbon or alloy steel and stainless steel. In addition, within the range of availability of information, the results of the evaluation were compared with the results from the various decommissioning experiences data or international/national decommissioning study. The comparison results have shown that the radioactive waste amount from Kori Unit 1 decommissioning were much less than those from the plants decommissioned in U.S. and were comparable to those from the plants in Europe. This result comes from the difference of disposal cost and clearance criteria (i.e., free release level) between U.S. and non-U.S. The preliminary evaluation performed using the methodology established in this study will be useful as a important information in establishing the decommissioning planning for the decommissioning schedule and waste management strategy establishment including the transportation, packaging, handling, and disposal of radioactive wastes.

Keywords: characterization, classification, decommissioning, decontamination and dismantling, Kori 1, radioactive waste

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55 Cleaning of Polycyclic Aromatic Hydrocarbons (PAH) Obtained from Ferroalloys Plant

Authors: Stefan Andersson, Balram Panjwani, Bernd Wittgens, Jan Erik Olsen

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Polycyclic Aromatic hydrocarbons are organic compounds consisting of only hydrogen and carbon aromatic rings. PAH are neutral, non-polar molecules that are produced due to incomplete combustion of organic matter. These compounds are carcinogenic and interact with biological nucleophiles to inhibit the normal metabolic functions of the cells. Norways, the most important sources of PAH pollution is considered to be aluminum plants, the metallurgical industry, offshore oil activity, transport, and wood burning. Stricter governmental regulations regarding emissions to the outer and internal environment combined with increased awareness of the potential health effects have motivated Norwegian metal industries to increase their efforts to reduce emissions considerably. One of the objective of the ongoing industry and Norwegian research council supported "SCORE" project is to reduce potential PAH emissions from an off gas stream of a ferroalloy furnace through controlled combustion. In a dedicated combustion chamber. The sizing and configuration of the combustion chamber depends on the combined properties of the bulk gas stream and the properties of the PAH itself. In order to achieve efficient and complete combustion the residence time and minimum temperature need to be optimized. For this design approach reliable kinetic data of the individual PAH-species and/or groups thereof are necessary. However, kinetic data on the combustion of PAH are difficult to obtain and there is only a limited number of studies. The paper presents an evaluation of the kinetic data for some of the PAH obtained from literature. In the present study, the oxidation is modelled for pure PAH and also for PAH mixed with process gas. Using a perfectly stirred reactor modelling approach the oxidation is modelled including advanced reaction kinetics to study influence of residence time and temperature on the conversion of PAH to CO2 and water. A Chemical Reactor Network (CRN) approach is developed to understand the oxidation of PAH inside the combustion chamber. Chemical reactor network modeling has been found to be a valuable tool in the evaluation of oxidation behavior of PAH under various conditions.

Keywords: PAH, PSR, energy recovery, ferro alloy furnace

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54 The Microstructure and Corrosion Behavior of High Entropy Metallic Layers Electrodeposited by Low and High-Temperature Methods

Authors: Zbigniew Szklarz, Aldona Garbacz-Klempka, Magdalena Bisztyga-Szklarz

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Typical metallic alloys bases on one major alloying component, where the addition of other elements is intended to improve or modify certain properties, most of all the mechanical properties. However, in 1995 a new concept of metallic alloys was described and defined. High Entropy Alloys (HEA) contains at least five alloying elements in an amount from 5 to 20 at.%. A common feature this type of alloys is an absence of intermetallic phases, high homogeneity of the microstructure and unique chemical composition, what leads to obtaining materials with very high strength indicators, stable structures (also at high temperatures) and excellent corrosion resistance. Hence, HEA can be successfully used as a substitutes for typical metallic alloys in various applications where a sufficiently high properties are desirable. For fabricating HEA, a few ways are applied: 1/ from liquid phase i.e. casting (usually arc melting); 2/ from solid phase i.e. powder metallurgy (sintering methods preceded by mechanical synthesis) and 3/ from gas phase e.g. sputtering or 4/ other deposition methods like electrodeposition from liquids. Application of different production methods creates different microstructures of HEA, which can entail differences in their properties. The last two methods also allows to obtain coatings with HEA structures, hereinafter referred to as High Entropy Films (HEF). With reference to above, the crucial aim of this work was the optimization of the manufacturing process of the multi-component metallic layers (HEF) by the low- and high temperature electrochemical deposition ( ED). The low-temperature deposition process was crried out at ambient or elevated temperature (up to 100 ᵒC) in organic electrolyte. The high-temperature electrodeposition (several hundred Celcius degrees), in turn, allowed to form the HEF layer by electrochemical reduction of metals from molten salts. The basic chemical composition of the coatings was CoCrFeMnNi (known as Cantor’s alloy). However, it was modified by other, selected elements like Al or Cu. The optimization of the parameters that allow to obtain as far as it possible homogeneous and equimolar composition of HEF is the main result of presented studies. In order to analyse and compare the microstructure, SEM/EBSD, TEM and XRD techniques were employed. Morover, the determination of corrosion resistance of the CoCrFeMnNi(Cu or Al) layers in selected electrolytes (i.e. organic and non-organic liquids) was no less important than the above mentioned objectives.

Keywords: high entropy alloys, electrodeposition, corrosion behavior, microstructure

Procedia PDF Downloads 81
53 Free-Standing Pd-Based Metallic Glass Membranes for MEMS Applications

Authors: Wei-Shan Wang, Klaus Vogel, Felix Gabler, Maik Wiemer, Thomas Gessner

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Metallic glasses, which are free of grain boundaries, have superior properties including large elastic limits, high strength, and excellent wear and corrosion resistance. Therefore, bulk metallic glasses (BMG) and thin film metallic glasses (TFMG) have been widely developed and investigated. Among various kinds of metallic glasses, Pd-Cu-Si TFMG, which has lower elastic modulus and better resistance of oxidation and corrosions compared to Zr- and Fe-based TFMGs, can be a promising candidate for MEMS applications. However, the study of Pd-TFMG membrane is still limited. This paper presents free-standing Pd-based metallic glass membranes with large area fabricated on wafer level for the first time. Properties of Pd-Cu-Si thin film metallic glass (TFMG) with various deposition parameters are investigated first. When deposited at 25°C, compressive stress occurs in the Pd76Cu6Si18 thin film regardless of Ar pressure. When substrate temperature is increased to 275°C, the stress state changes from compressive to tensile. Thin film stresses are slightly decreased when Ar pressure is higher. To show the influence of temperature on Pd-TFMGs, thin films without and with post annealing below (275°C) and within (370°C) supercooled liquid region are investigated. Results of XRD and TEM analysis indicate that Pd-TFMGs remain amorphous structure with well-controlled parameters. After verification of amorphous structure of the Pd-TFMGs, free-standing Pd-Cu-Si membranes were fabricated by depositing Pd-Cu-Si thin films directly on 200nm-thick silicon nitride membranes, followed by post annealing and dry etching of silicon nitride layer. Post annealing before SiNx removal is used to further release internal stress of Pd-TFMGs. The edge length of the square membrane ranges from 5 to 8mm. The effect of post annealing on Pd-Cu-Si membranes are discussed as well. With annealing at 370°C for 5 min, Pd-MG membranes are fully distortion-free after removal of SiNx layer. Results show that, by introducing annealing process, the stress-relief, distortion-free Pd-TFMG membranes with large area can be a promising candidate for sensing applications such as pressure and gas sensors.

Keywords: amorphous alloy, annealing, metallic glasses, TFMG membrane

Procedia PDF Downloads 352
52 Analysis of Superconducting and Optical Properties in Atomic Layer Deposition and Sputtered Thin Films for Next-Generation Single-Photon Detectors

Authors: Nidhi Choudhary, Silke A. Peeters, Ciaran T. Lennon, Dmytro Besprozvannyy, Harm C. M. Knoops, Robert H. Hadfield

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Superconducting Nanowire Single Photon Detectors (SNSPDs) have become leading devices in quantum optics and photonics, known for their exceptional efficiency in detecting single photons from ultraviolet to mid-infrared wavelengths with minimal dark counts, low noise, and reduced timing jitter. Recent advancements in materials science focus attention on refractory metal thin films such as NbN and NbTiN to enhance the optical properties and superconducting performance of SNSPDs, opening the way for next-generation detectors. These films have been deposited by several different techniques, such as atomic layer deposition (ALD), plasma pro-advanced plasma processing (ASP) and magnetron sputtering. The fabrication flexibility of these films enables precise control over morphology, crystallinity, stoichiometry and optical properties, which is crucial for optimising the SNSPD performance. Hence, it is imperative to study the optical and superconducting properties of these materials across a wide range of wavelengths. This study provides a comprehensive analysis of the optical and superconducting properties of some important materials in this category (NbN, NbTiN) by different deposition methods. Using Variable angle ellipsometry spectroscopy (VASE), we measured the refractive index, extinction, and absorption coefficient across a wide wavelength range (200-1700 nm) to enhance light confinement for optical communication devices. The critical temperature and sheet resistance were measured using a four-probe method in a custom-built, cryogen-free cooling system with a Sumitomo RDK-101D cold head and CNA-11C compressor. Our results indicate that ALD-deposited NbN shows a higher refractive index and extinction coefficient in the near-infrared region (~1500 nm) than sputtered NbN of the same thickness. Further, the analysis of the optical properties of plasma pro-ASP deposited NbTiN was performed at different substrate bias voltages and different thicknesses. The analysis of substrate bias voltage indicates that the maximum value of the refractive index and extinction coefficient observed for the substrate biasing of 50-80 V across a substrate bias range of (0 V - 150 V). The optical properties of sputtered NbN films are also investigated in terms of the different substrate temperatures during deposition (100 °C-500 °C). We find the higher the substrate temperature during deposition, the higher the value of the refractive index and extinction coefficient has been observed. In all our superconducting thin films ALD-deposited NbN films possess the highest critical temperature (~12 K) compared to sputtered (~8 K) and plasma pro-ASP (~5 K).

Keywords: optical communication, thin films, superconductivity, atomic layer deposition (ALD), niobium nitride (NbN), niobium titanium nitride (NbTiN), SNSPD, superconducting detector, photon-counting.

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51 Structure and Properties of Intermetallic NiAl-Based Coatings Produced by Magnetron Sputtering Technique

Authors: Tatiana S. Ogneva

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Aluminum and nickel-based intermetallic compounds have attracted the attention of scientific community as promising materials for heat-resistant and wear-resistant coatings in such manufacturing areas as microelectronics, aircraft and rocket building and chemical industries. Magnetron sputtering makes possible to coat materials without formation of liquid phase and improves the mechanical and functional properties of nickel aluminides due to the possibility of nanoscale structure formation. The purpose of the study is the investigation of structure and properties of intermetallic coatings produced by magnetron sputtering technique. The feature of this work is the using of composite targets for sputtering, which were consisted of two semicircular sectors of cp-Ni and cp-Al. Plates of alumina, silicon, titanium and steel alloys were used as substrates. To estimate sputtering conditions on structure of intermetallic coatings, a series of samples were produced and studied in detail using scanning and transition electron microcopy and X-Ray diffraction. Besides, nanohardness and scratching tests were carried out. The varying parameters were the distance from the substrate to the target, the duration and the power of the sputtering. The thickness of the obtained intermetallic coatings varied from 0.05 to 0.5 mm depending on the sputtering conditions. The X-ray diffraction data indicated that the formation of intermetallic compounds occurred after sputtering without additional heat treatment. Sputtering at a distance not closer than 120 mm led to the formation of NiAl phase. Increase in the power of magnetron from 300 to 900 W promoted the increase of heterogeneity of the phase composition and the appearance of intermetallic phases NiAl, Ni₂Al₃, NiAl₃, and Al under the aluminum side, and NiAl, Ni₃Al, and Ni under the nickel side of the target. A similar trend is observed with increasing the distance of sputtering from 100 to 60 mm. The change in the phase composition correlates with the changing of the atomic composition of the coatings. Scanning electron microscopy revealed that the coatings have a nanoscale grain structure. In this case, the substrate material and the distance from the substrate to the magnetron have a significant effect on the structure formation process. The size of nanograins differs from 10 to 83 nm and depends not only on the sputtering modes but also on material of a substrate. Nanostructure of the material influences the level of mechanical properties. The highest level of nanohardness of the coatings deposited during 30 minutes on metallic substrates at a distance of 100 mm reached 12 GPa. It was shown that nanohardness depends on the grain size of the intermetallic compound. Scratching tests of the coatings showed a high level of adhesion of the coating to substrate without any delamination and cracking. The results of the study showed that magnetron sputtering of composite targets consisting of nickel and aluminum semicircles makes it possible to form intermetallic coatings with good mechanical properties directly in the process of sputtering without additional heat treatment.

Keywords: intermetallic coatings, magnetron sputtering, mechanical properties, structure

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50 The Creation of Calcium Phosphate Coating on Nitinol Substrate

Authors: Kirill M. Dubovikov, Ekaterina S. Marchenko, Gulsharat A. Baigonakova

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NiTi alloys are widely used as implants in medicine due to their unique properties such as superelasticity, shape memory effect and biocompatibility. However, despite these properties, one of the major problems is the release of nickel after prolonged use in the human body under dynamic stress. This occurs due to oxidation and cracking of NiTi implants, which provokes nickel segregation from the matrix to the surface and release into living tissues. As we know, nickel is a toxic element and can cause cancer, allergies, etc. One of the most popular ways to solve this problem is to create a corrosion resistant coating on NiTi. There are many coatings of this type, but not all of them have good biocompatibility, which is very important for medical implants. Coatings based on calcium phosphate phases have excellent biocompatibility because Ca and P are the main constituents of the mineral part of human bone. This fact suggests that a Ca-P coating on NiTi can enhance osteogenesis and accelerate the healing process. Therefore, the aim of this study is to investigate the structure of Ca-P coating on NiTi substrate. Plasma assisted radio frequency (RF) sputtering was used to obtain this film. This method was chosen because it allows the crystallinity and morphology of the Ca-P coating to be controlled by the sputtering parameters. It allows us to obtain three different NiTi samples with Ca-P coating. XRD, AFM, SEM and EDS were used to study the composition, structure and morphology of the coating phase. Scratch tests were carried out to evaluate the adhesion of the coating to the substrate. Wettability tests were used to investigate the hydrophilicity of the different coatings and to suggest which of them had better biocompatibility. XRD showed that the coatings of all samples were hydroxyapatite, but the matrix was represented by TiNi intermetallic compounds such as B2, Ti2Ni and Ni3Ti. The SEM shows that the densest and defect-free coating has only one sample after three hours of sputtering. Wettability tests show that the sample with the densest coating has the lowest contact angle of 40.2° and the largest free surface area of 57.17 mJ/m2, which is mostly disperse. A scratch test was carried out to investigate the adhesion of the coating to the surface and it was shown that all coatings were removed by a cohesive mechanism. However, at a load of 30N, the indenter reached the substrate in two out of three samples, except for the sample with the densest coating. It was concluded that the most promising sputtering mode was the third, which consisted of three hours of deposition. This mode produced a defect-free Ca-P coating with good wettability and adhesion.

Keywords: biocompatibility, calcium phosphate coating, NiTi alloy, radio frequency sputtering.

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49 The Effect of TiO₂ Nanoparticles on Zebrafish Embryos

Authors: Elena Maria Scalisi

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Currently, photodegradation by nanoparticles (NPs) is a common solution for wastewater treatment. Nanoparticles are efficient for removing organic and inorganic pollutants, heavy metals from wastewater and killing microorganisms through environmentally friendly. In this context, the major representative of photocatalytic technology for industrial wastewater treatment are TiO₂ nanoparticles (TiO₂-NPs). TiO₂-NPs have a strong catalytic activity that depends to their physicochemical properties. Thanks to their small size (between 1-100 nm), nanoparticles occupy less volume, then their surface area increases. The increase in the surface-to-volume ratio results in the increase of the particle surface energy, which improve their reactivity potential. However, these unique properties represent risks to the ecosystems and organisms when unintentionally TiO₂-NPs are release into the environment and absorbed by living organisms. Several studies confirm that there is a high level of interest concerning the safety of TiO₂-NPs in the aquatic environment, furthermore, ecotoxicological tools are useful to correctly evaluate their toxicity. In the current study, we aimed to characterize potential toxic effects of TiO₂-NP suspension to zebrafish during embryo-larval stages to evaluate parameters such as survival rates, malformation, hatching, the overall length of the larvae heartbeat, and biochemical biomarkers that reflect the acute toxicity and sublethal effects of TiO₂-NPs. Zebrafish embryos were exposed to titanium dioxide nanoparticles (TiO₂-NPs at 1mg/L, 2mg/L, and 4mg/L) from fertilization to the free swimming stage (144hpf). Every day, we recorded the toxicological endpoints, moreover, immunohistochemical analysis has been performed at the end of the exposure. In particular, we have evaluate the expression of the following biomarkers: Heat Shock Protein 70 (HSP70), Poly ADP-Ribose Polymerase-1 (PARP-1), Metallothioneins (MTs). Our results have shown that hatch ability, survival, and malformation rate were not affected by TiO₂ NPs at these exposure levels. However, TiO₂-NPs caused an increase of heartbeat and reduction of body length; at the same time, TiO₂-NPs have inducted the production of ROS and the expression of oxidative stress biomarkers HSP70 and PARP-1. Hight positivity for PARP-1 at all concentration tested was observed. As regards MT, positivity was found in the expression of this biomarker in the whole body of the embryo, with the exception of the end of the tail. Metallothioneins (MT) are biomarkers widely used in environmental monitoring programs for aquatic creatures. At the light of our results i.e. no death until the end of the experiment (144hpf), no malformation and expression of the biomarkers mentioned, it is evident that zebrafish larvae with their natural detoxification pathways are able to resist the presence of toxic substances and then they can tolerate the presence of metal concentrations. However, an excessive oxidative state can compromise cell function, therefore the uncontrolled release of nanoparticles into the environment is severe and must be constantly monitored.

Keywords: nanoparticles, embryo zebrafish, HSP70, PARP-1

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48 Performance of HVOF Sprayed Ni-20CR and Cr3C2-NiCr Coatings on Fe-Based Superalloy in an Actual Industrial Environment of a Coal Fired Boiler

Authors: Tejinder Singh Sidhu

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Hot corrosion has been recognized as a severe problem in steam-powered electricity generation plants and industrial waste incinerators as it consumes the material at an unpredictably rapid rate. Consequently, the load-carrying ability of the components reduces quickly, eventually leading to catastrophic failure. The inability to either totally prevent hot corrosion or at least detect it at an early stage has resulted in several accidents, leading to loss of life and/or destruction of infrastructures. A number of countermeasures are currently in use or under investigation to combat hot corrosion, such as using inhibitors, controlling the process parameters, designing a suitable industrial alloy, and depositing protective coatings. However, the protection system to be selected for a particular application must be practical, reliable, and economically viable. Due to the continuously rising cost of the materials as well as increased material requirements, the coating techniques have been given much more importance in recent times. Coatings can add value to products up to 10 times the cost of the coating. Among the different coating techniques, thermal spraying has grown into a well-accepted industrial technology for applying overlay coatings onto the surfaces of engineering components to allow them to function under extreme conditions of wear, erosion-corrosion, high-temperature oxidation, and hot corrosion. In this study, the hot corrosion performances of Ni-20Cr and Cr₃C₂-NiCr coatings developed by High Velocity Oxy-Fuel (HVOF) process have been studied. The coatings were developed on a Fe-based superalloy, and experiments were performed in an actual industrial environment of a coal-fired boiler. The cyclic study was carried out around the platen superheater zone where the temperature was around 1000°C. The study was conducted for 10 cycles, and one cycle was consisting of 100 hours of heating followed by 1 hour of cooling at ambient temperature. Both the coatings deposited on Fe-based superalloy imparted better hot corrosion resistance than the uncoated one. The Ni-20Cr coated superalloy performed better than the Cr₃C₂-NiCr coated in the actual working conditions of the coal fired boiler. It is found that the formation of chromium oxide at the boundaries of Ni-rich splats of the coating blocks the inward permeation of oxygen and other corrosive species to the substrate.

Keywords: hot corrosion, coating, HVOF, oxidation

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47 Effect of Ti, Nb, and Zr Additives on Biocompatibility of Injection Molded 316L Stainless Steel for Biomedical Applications

Authors: Busra Gundede, Ozal Mutlu, Nagihan Gulsoy

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Background: Over the years, material research has led to the development of numerous metals and alloys for using in biomedical applications. One of the major tasks of biomaterial research is the functionalization of the material surface to improve the biocompatibility according to a specific application. 316L and 316L alloys are excellent for various bio-applications. This research was investigated the effect of titanium (Ti), niobium (Nb), and zirconium (Zr) additives on injection molded austenitic grade 316L stainless steels in vitro biocompatibility. For this purpose, cytotoxic tests were performed to evaluate the potential biocompatibility of the specimens. Materials and Methods: 3T3 fibroblast were cultivated in DMEM supplemented with 10% fetal bovine serum and %1 penicillin-streptomycin at 37°C with 5% CO2 and 95%humidity. Trypsin/EDTA solution was used to remove cells from the culture flask. Cells were reseeded at a density of 1×105cell in 25T flasks. The medium change took place every 3 days. The trypan blue assay was used to determine cell viability. Cell viability is calculated as the number of viable cells divided by the total number of cells within the grids on the cell counter machine counted the number of blue staining cells and the number of total cells. Cell viability should be at least 95% for healthy log-phase cultures. MTT assay was assessed for 96-hours. Cells were cultivated in 6-well flask within 5 ml DMEM and incubated as same conditions. 0,5mg/ml MTT was added for 4-hours and then acid-isoprohanol was added for solubilize to formazan crystals. Cell morphology after 96h was investigated by SEM. The medium was removed, samples were washed with 0.15 M PBS buffer and fixed for 12h at 4- 8°C with %2,5 gluteraldehyte. Samples were treated with 1% osmium tetroxide. Samples were then dehydrated and dried, mounted on appropriate stubs with colloidal silver and sputter-coated with gold. Images were collected using a scanning electron microscope. ROS assay is a cell viability test for in vitro studies. Cells were grown for 96h, ROS solution added on cells in 6 well plate flask and incubated for 1h. Fluorescence signal indicates ROS generation by cells. Results: Trypan Blue exclusion assay results were 96%, 92%, 95%, 90%, 91% for negative control group, 316L, 316L-Ti, 316L-Nb and 316L-Zr, respectively. Results were found nearly similar to each other when compared with control group. Cell viability from MTT analysis was found to be 100%, 108%, 103%, 107%, and 105% for the control group, 316L, 316L-Ti, 316L-Nb and 316L-Zr, respectively. Fluorescence microscopy analysis indicated that all test groups were same as the control group in ROS assay. SEM images demonstrated that the attachment of 3T3 cells on biomaterials. Conclusion: We, therefore, concluded that Ti, Nb and Zr additives improved physical properties of 316L stainless. In our in vitro experiments showed that these new additives did not modify the cytocompatibility of stainless steel and these additives on 316L might be useful for biomedical applications.

Keywords: 316L stainles steel, biocompatibility, cell culture, Ti, Nb, Zr

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46 Blade-Coating Deposition of Semiconducting Polymer Thin Films: Light-To-Heat Converters

Authors: M. Lehtihet, S. Rosado, C. Pradère, J. Leng

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Poly(3,4-ethylene dioxythiophene) polystyrene sulfonate (PEDOT: PSS), is a polymer mixture well-known for its semiconducting properties and is widely used in the coating industry for its visible transparency and high electronic conductivity (up to 4600 S/cm) as a transparent non-metallic electrode and in organic light-emitting diodes (OLED). It also possesses strong absorption properties in the Near Infra-Red (NIR) range (λ ranging between 900 nm to 2.5 µm). In the present work, we take advantage of this absorption to explore its potential use as a transparent light-to-heat converter. PEDOT: PSS aqueous dispersions are deposited onto a glass substrate using a blade-coating technique in order to produce uniform coatings with controlled thicknesses ranging in ≈ 400 nm to 2 µm. Blade-coating technique allows us good control of the deposit thickness and uniformity by the tuning of several experimental conditions (blade velocity, evaporation rate, temperature, etc…). This liquid coating technique is a well-known, non-expensive technique to realize thin film coatings on various substrates. For coatings on glass substrates destined to solar insulation applications, the ideal coating would be made of a material able to transmit all the visible range while reflecting the NIR range perfectly, but materials possessing similar properties still have unsatisfactory opacity in the visible too (for example, titanium dioxide nanoparticles). NIR absorbing thin films is a more realistic alternative for such an application. Under solar illumination, PEDOT: PSS thin films heat up due to absorption of NIR light and thus act as planar heaters while maintaining good transparency in the visible range. Whereas they screen some NIR radiation, they also generate heat which is then conducted into the substrate that re-emits this energy by thermal emission in every direction. In order to quantify the heating power of these coatings, a sample (coating on glass) is placed in a black enclosure and illuminated with a solar simulator, a lamp emitting a calibrated radiation very similar to the solar spectrum. The temperature of the rear face of the substrate is measured in real-time using thermocouples and a black-painted Peltier sensor measures the total entering flux (sum of transmitted and re-emitted fluxes). The heating power density of the thin films is estimated from a model of the thin film/glass substrate describing the system, and we estimate the Solar Heat Gain Coefficient (SHGC) to quantify the light-to-heat conversion efficiency of such systems. Eventually, the effect of additives such as dimethyl sulfoxide (DMSO) or optical scatterers (particles) on the performances are also studied, as the first one can alter the IR absorption properties of PEDOT: PSS drastically and the second one can increase the apparent optical path of light within the thin film material.

Keywords: PEDOT: PSS, blade-coating, heat, thin-film, Solar spectrum

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45 The Role of Nickel on the High-Temperature Corrosion of Modell Alloys (Stainless Steels) before and after Breakaway Corrosion at 600°C: A Microstructural Investigation

Authors: Imran Hanif, Amanda Persdotter, Sedigheh Bigdeli, Jesper Liske, Torbjorn Jonsson

Abstract:

Renewable fuels such as biomass/waste for power production is an attractive alternative to fossil fuels in order to achieve a CO₂ -neutral power generation. However, the combustion results in the release of corrosive species. This puts high demands on the corrosion resistance of the alloys used in the boiler. Stainless steels containing nickel and/or nickel containing coatings are regarded as suitable corrosion resistance material especially in the superheater regions. However, the corrosive environment in the boiler caused by the presence of water vapour and reactive alkali very rapidly breaks down the primary protection, i.e., the Cr-rich oxide scale formed on stainless steels. The lifetime of the components, therefore, relies on the properties of the oxide scale formed after breakaway, i.e., the secondary protection. The aim of the current study is to investigate the role of varying nickel content (0–82%) on the high-temperature corrosion of model alloys with 18% Cr (Fe in balance) in the laboratory mimicking industrial conditions at 600°C. The influence of nickel is investigated on both the primary protection and especially the secondary protection, i.e., the scale formed after breakaway, during the oxidation/corrosion process in the dry O₂ (primary protection) and more aggressive environment such as H₂O, K₂CO₃ and KCl (secondary protection). All investigated alloys experience a very rapid loss of the primary protection, i.e., the Cr-rich (Cr, Fe)₂O₃, and the formation of secondary protection in the aggressive environments. The microstructural investigation showed that secondary protection of all alloys has a very similar microstructure in all more aggressive environments consisting of an outward growing iron oxide and inward growing spinel-oxide (Fe, Cr, Ni)₃O₄. The oxidation kinetics revealed that it is possible to influence the protectiveness of the scale formed after breakaway (secondary protection) through the amount of nickel in the alloy. The difference in oxidation kinetics of the secondary protection is linked to the microstructure and chemical composition of the complex spinel-oxide. The detailed microstructural investigations were carried out using the extensive analytical techniques such as electron back scattered diffraction (EBSD), energy dispersive X-rays spectroscopy (EDS) via the scanning and transmission electron microscopy techniques and results are compared with the thermodynamic calculations using the Thermo-Calc software.

Keywords: breakaway corrosion, EBSD, high-temperature oxidation, SEM, TEM

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44 Estimation of Morbidity Level of Industrial Labour Conditions at Zestafoni Ferroalloy Plant

Authors: M. Turmanauli, T. Todua, O. Gvaberidze, R. Javakhadze, N. Chkhaidze, N. Khatiashvili

Abstract:

Background: Mining process has the significant influence on human health and quality of life. In recent years the events in Georgia were reflected on the industry working process, especially minimal requirements of labor safety, hygiene standards of workplace and the regime of work and rest are not observed. This situation is often caused by the lack of responsibility, awareness, and knowledge both of workers and employers. The control of working conditions and its protection has been worsened in many of industries. Materials and Methods: For evaluation of the current situation the prospective epidemiological study by face to face interview method was conducted at Georgian “Manganese Zestafoni Ferroalloy Plant” in 2011-2013. 65.7% of employees (1428 bulletin) were surveyed and the incidence rates of temporary disability days were studied. Results: The average length of a temporary disability single accident was studied taking into consideration as sex groups as well as the whole cohort. According to the classes of harmfulness the following results were received: Class 2.0-10.3%; 3.1-12.4%; 3.2-35.1%; 3.3-12.1%; 3.4-17.6%; 4.0-12.5%. Among the employees 47.5% and 83.1% were tobacco and alcohol consumers respectively. According to the age groups and years of work on the base of previous experience ≥50 ages and ≥21 years of work data prevalence respectively. The obtained data revealed increased morbidity rate according to age and years of work. It was found that the bone and articulate system and connective tissue diseases, aggravation of chronic respiratory diseases, ischemic heart diseases, hypertension and cerebral blood discirculation were the leading among the other diseases. High prevalence of morbidity observed in the workplace with not satisfactory labor conditions from the hygienic point of view. Conclusion: According to received data the causes of morbidity are the followings: unsafety labor conditions; incomplete of preventive medical examinations (preliminary and periodic); lack of access to appropriate health care services; derangement of gathering, recording, and analysis of morbidity data. This epidemiological study was conducted at the JSC “Manganese Ferro Alloy Plant” according to State program “ Prevention of Occupational Diseases” (Program code is 35 03 02 05).

Keywords: occupational health, mining process, morbidity level, cerebral blood discirculation

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43 The Challenges of Well Integrity on Plug and Abandoned Wells for Offshore Co₂ Storage Site Containment

Authors: Siti Noor Syahirah Mohd Sabri

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The oil and gas industry is committed to net zero carbon emissions because the consequences of climate change could be catastrophic unless responded to very soon. One way of reducing CO₂ emissions is to inject it into a depleted reservoir buried underground. This greenhouse gas reduction technique significantly reduces CO₂ released into the atmosphere. In general, depleted oil and gas reservoirs provide readily available sites for the storage of CO₂ in offshore areas. This is mainly due to the hydrocarbons have been optimally produced and the existence of voids for effective CO₂ storage. Hence, make it a good candidate for a CO₂ well injector location. Geological storage sites are often evaluated in terms of capacity, injectivity and containment. Leakage through the cap rock or existing well is the main concern in the depleted fields. In order to develop these fields as CO₂ storage sites, the long-term integrity of wells drilled in these oil & gas fields must be ascertained to ensure good CO₂ containment. Well, integrity is often defined as the ability to contain fluids without significant leakage through the project lifecycle. Most plugged and abandoned (P & A) wells in Peninsular Malaysia have drilled 20 – 30 years ago and were not designed to withstand downhole conditions having >50%vol CO₂ and CO₂/H₂O mixture. In addition, Corrosive-Resistant Alloy (CRA) tubular and CO₂-resistant cement was not used during good construction. The reservoir pressure and temperature conditions may have further degraded the material strength and elevated the corrosion rate. Understanding all the uncertainties that may have affected cement-casing bonds, such as the quality of cement behind the casing, subsidence effect, corrosion rate, etc., is the first step toward well integrity evaluation. Secondly, proper quantification of all the uncertainties involved needs to be done to ensure long-term underground storage objectives of CO₂ are achieved. This paper will discuss challenges associated with estimating the performance of well barrier elements in existing P&A wells. Risk ranking of the existing P&A wells is to be carried out in order to ensure the integrity of the storage site is maintained for long-term CO₂ storage. High-risk existing P&A wells are to be re-entered to restore good integrity and to reduce future leakage that may happen. In addition, the requirement to design a fit-for-purpose monitoring and mitigation technology package for potential CO₂ leakage/seepage in the marine environment will be discussed accordingly. The holistic approach will ensure that the integrity is maintained, and CO₂ is contained underground for years to come.

Keywords: CCUS, well integrity, co₂ storage, offshore

Procedia PDF Downloads 91
42 Temperature Dependent Magneto-Transport Properties of MnAl Binary Alloy Thin Films

Authors: Vineet Barwal, Sajid Husain, Nanhe Kumar Gupta, Soumyarup Hait, Sujeet Chaudhary

Abstract:

High perpendicular magnetic anisotropy (PMA) and low damping constant (α) in ferromagnets are one of the few necessary requirements for their potential applications in the field of spintronics. In this regards, ferromagnetic τ-phase of MnAl possesses the highest PMA (Ku > 107 erg/cc) at room temperature, high saturation magnetization (Ms~800 emu/cc) and a Curie temperature of ~395K. In this work, we have investigated the magnetotransport behaviour of this potentially useful binary system MnₓAl₁₋ₓ films were synthesized by co-sputtering (pulsed DC magnetron sputtering) on Si/SiO₂ (where SiO₂ is native oxide layer) substrate using 99.99% pure Mn and Al sputtering targets. Films of constant thickness (~25 nm) were deposited at the different growth temperature (Tₛ) viz. 30, 300, 400, 500, and 600 ºC with a deposition rate of ~5 nm/min. Prior to deposition, the chamber was pumped down to a base pressure of 2×10⁻⁷ Torr. During sputtering, the chamber was maintained at a pressure of 3.5×10⁻³ Torr with the 55 sccm Ar flow rate. Films were not capped for the purpose of electronic transport measurement, which leaves a possibility of metal oxide formation on the surface of MnAl (both Mn and Al have an affinity towards oxide formation). In-plane and out-of-plane transverse magnetoresistance (MR) measurements on films sputtered under optimized growth conditions revealed non-saturating behavior with MR values ~6% and 40% at 9T, respectively at 275 K. Resistivity shows a parabolic dependence on the field H, when the H is weak. At higher H, non-saturating positive MR that increases exponentially with the strength of magnetic field is observed, a typical character of hopping type conduction mechanism. An anomalous decrease in MR is observed on lowering the temperature. From the temperature dependence of reistivity, it is inferred that the two competing states are metallic and semiconducting, respectively and the energy scale of the phenomenon produces the most interesting effects, i.e., the metal-insulator transition and hence the maximum sensitivity to external fields, at room temperature. Theory of disordered 3D systems effectively explains the crossover temperature coefficient of resistivity from positive to negative with lowering of temperature. These preliminary findings on the MR behavior of MnAl thin films will be presented in detail. The anomalous large MR in mixed phase MnAl system is evidently useful for future spintronic applications.

Keywords: magnetoresistance, perpendicular magnetic anisotropy, spintronics, thin films

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41 Assessment of Heavy Metals Contamination Levels in Groundwater: A Case Study of the Bafia Agricultural Area, Centre Region Cameroon

Authors: Carine Enow-Ayor Tarkang, Victorine Neh Akenji, Dmitri Rouwet, Jodephine Njdma, Andrew Ako Ako, Franco Tassi, Jules Remy Ngoupayou Ndam

Abstract:

Groundwater is the major water resource in the whole of Bafia used for drinking, domestic, poultry and agricultural purposes, and being an area of intense agriculture, there is a great necessity to do a quality assessment. Bafia is one of the main food suppliers in the Centre region of Cameroon, and so to meet their demands, the farmers make use of fertilizers and other agrochemicals to increase their yield. Less than 20% of the population in Bafia has access to piped-borne water due to the national shortage, according to the authors best knowledge very limited studies have been carried out in the area to increase awareness of the groundwater resources. The aim of this study was to assess heavy metal contamination levels in ground and surface waters and to evaluate the effects of agricultural inputs on water quality in the Bafia area. 57 water samples (including 31 wells, 20 boreholes, 4 rivers and 2 springs) were analyzed for their physicochemical parameters, while collected samples were filtered, acidified with HNO3 and analyzed by ICP-MS for their heavy metal content (Fe, Ti, Sr, Al, Mn). Results showed that most of the water samples are acidic to slightly neutral and moderately mineralized. Ti concentration was significantly high in the area (mean value 130µg/L), suggesting another Ti source besides the natural input from Titanium oxides. The high amounts of Mn and Al in some cases also pointed to additional input, probably from fertilizers that are used in the farmlands. Most of the water samples were found to be significantly contaminated with heavy metals exceeding the WHO allowable limits (Ti-94.7%, Al-19.3%, Mn-14%, Fe-5.2% and Sr-3.5% above limits), especially around farmlands and topographic low areas. The heavy metal concentration was evaluated using the heavy metal pollution index (HPI), heavy metal evaluation index (HEI) and degree of contamination (Cd), while the Ficklin diagram was used for the water based on changes in metal content and pH. The high mean values of HPI and Cd (741 and 5, respectively), which exceeded the critical limit, indicate that the water samples are highly contaminated, with intense pollution from Ti, Al and Mn. Based on the HPI and Cd, 93% and 35% of the samples, respectively, are unacceptable for drinking purposes. The lowest HPI value point also had the lowest EC (50 µS/cm), indicating lower mineralization and less anthropogenic influence. According to the Ficklin diagram, 89% of the samples fell within the near-neutral low-metal domain, while 9% fell in the near-neutral extreme-metal domain. Two significant factors were extracted from the PCA, explaining 70.6% of the total variance. The first factor revealed intense anthropogenic activity (especially from fertilizers), while the second factor revealed water-rock interactions. Agricultural activities thus have an impact on the heavy metal content of groundwater in the area; hence, much attention should be given to the affected areas in order to protect human health/life and thus sustainably manage this precious resource.

Keywords: Bafia, contamination, degree of contamination, groundwater, heavy metal pollution index

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40 Bioleaching of Precious Metals from an Oil-fired Ash Using Organic Acids Produced by Aspergillus niger in Shake Flasks and a Bioreactor

Authors: Payam Rasoulnia, Seyyed Mohammad Mousavi

Abstract:

Heavy fuel oil firing power plants produce huge amounts of ashes as solid wastes, which seriously need to be managed and processed. Recycling precious metals of V and Ni from these oil-fired ashes which are considered as secondary sources of metals recovery, not only has a great economic importance for use in industry, but also it is noteworthy from the environmental point of view. Vanadium is an important metal that is mainly used in the steel industry because of its physical properties of hardness, tensile strength, and fatigue resistance. It is also utilized in oxidation catalysts, titanium–aluminum alloys and vanadium redox batteries. In the present study bioleaching of vanadium and nickel from an oil-fired ash sample was conducted using Aspergillus niger fungus. The experiments were carried out using spent-medium bioleaching method in both Erlenmeyer flasks and also bubble column bioreactor, in order to compare them together. In spent-medium bioleaching the solid waste is not in direct contact with the fungus and consequently the fungal growth is not retarded and maximum organic acids are produced. In this method the metals are leached through biogenic produced organic acids present in the medium. In shake flask experiments the fungus was cultured for 15 days, where the maximum production of organic acids was observed, while in bubble column bioreactor experiments a 7 days fermentation period was applied. The amount of produced organic acids were measured using high performance liquid chromatography (HPLC) and the results showed that depending on the fermentation period and the scale of experiments, the fungus has different major lixiviants. In flask tests, citric acid was the main produced organic acid by the fungus and the other organic acids including gluconic, oxalic, and malic were excreted in much lower concentrations, while in the bioreactor oxalic acid was the main lixiviant and it was produced considerably. In Erlenmeyer flasks during 15 days fermentation of Aspergillus niger, 8080 ppm citric acid and 1170 ppm oxalic acid was produced, while in bubble column bioreactor over 7 days of fungal growth, 17185 ppm oxalic acid and 1040 ppm citric acid was secreted. The leaching tests using the spent-media obtained from both of fermentation experiments, were performed at the same conditions of leaching duration of 7 days, leaching temperature of 60 °C and pulp density up to 3% (w/v). The results revealed that in Erlenmeyer flask experiments 97% of V and 50% of Ni were extracted while using spent medium produced in bubble column bioreactor, V and Ni recoveries were achieved to 100% and 33%, respectively. These recovery yields indicate that in both scales almost total vanadium can be recovered, while nickel recovery was lower. With help of the bioreactor spent-medium nickel recovery yield was lower than that of obtained from the flask experiments, which it could be due to precipitation of some values of Ni in presence of high levels of oxalic acid existing in its spent medium.

Keywords: Aspergillus niger, bubble column bioreactor, oil-fired ash, spent-medium bioleaching

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