Abstract: The refractory high entropy alloys are potential materials for high-temperature applications because of their ability to retain high strength up to 1600°C. However, their practical applications were limited due to poor elongation at room temperature. Therefore, decreasing the average valence electron concentrations (VEC) is an effective design strategy to improve the intrinsic ductility of refractory high entropy alloys. In this work, the high-entropy alloy TaNbHfZrTi was processed at room temperature by each step reverse rolling up to a 90% reduction in thickness. Subsequently, the reverse rolled 90% samples were utilized for annealing treatment at 800°C and 1000°C for 1 h to understand phase stability, microstructure, texture, and mechanical properties. The reverse rolled 90% condition contains body-centered cubic (BCC) single-phase; upon annealing at 800 °C, the formation of secondary phase BCC-2 prevailed. The partial recrystallization and complete recrystallization microstructures were developed for annealed at 800°C and 1000°C, respectively. The reverse rolled condition and 1000°C annealed temperature exhibit extraordinary room temperature tensile properties with high ultimate tensile strength (UTS) without compromising loss of ductility called “strength-ductility” trade-off. The reverse-rolled 90% and annealing treatment carried out at temperature about 1000°C for 1 h consist of UTS 1430 MPa and 1556 MPa with an appreciable amount of 21% and 20% elongation, respectively. The development of hierarchical microstructure prevailed for the annealed 1000°C which led to the simultaneous increase in tensile strength and elongation.
Abstract: The refractory alloys are crucial for high-temperature applications to improve performance and reduce cost. They are used in several applications such as aerospace, outer space, military and defense, nuclear powerplants, automobiles, and industry. The conventional refractory alloys show greater stability at high temperatures and in contrast they have operational limitations due to their low melting temperatures. However, there is a huge requirement to improve the refractory alloys’ operational temperatures and replace the conventional alloys. The newly emerging refractory high entropy alloys (RHEAs) could be alternative materials for conventional refractory alloys and fulfill the demands and requirements of various practical applications in the future. The RHEA TaHfNbZrTi was prepared through an arc melting process. The annealing behavior of severely deformed equiatomic RHEATaHfNbZrTi has been investigated. To obtain deformed condition, the alloy is cold-rolled to 90% thickness reduction and then subjected to an annealing process to observe recrystallization and microstructural evolution in the range of 800 °C to 1400 °C temperatures. The cold-rolled – 90% condition shows the presence of microstructural heterogeneity. The annealing microstructure of 800 °C temperature reveals that partial recrystallization and further annealing treatment carried out annealing treatment in the range of 850 °C to 1400 °C temperatures exhibits completely recrystallized microstructures, followed by coarsening with a degree of annealing temperature. The deformed and annealed conditions featured the development of body-centered cubic (BCC) fiber textures. The experimental investigation of heavy deformation and followed by high-temperature annealing up to 1400 °C temperature will contribute to the understanding of microstructure and texture evolution of emerging RHEAs.
Abstract: The γ-TiAl based Ti-Al-Mn-Nb alloys were fabricated
by selective laser melting (SLM) on the TC4 substrate. The
microstructures of the alloys were investigated in detail. The results
reveal that the alloy without electromagnetic stirring (EMS) consists
of γ-TiAl phase with tetragonal structure and α2-Ti3Al phase
with hcp structure, while the alloy with applied EMS consists of
γ-TiAl, α2-Ti3Al and α-Ti with hcp structure, and the morphological
structure of the alloy without EMS which exhibits near lamellar
structure and the alloy with EMS shows duplex structure, the alloy
without EMS shows some microcracks and pores while they are not
observed in the alloy without EMS. The microhardness and wear
resistance values decrease with applied EMS.
Abstract: In this present work, five different composite samples with AA2024 as matrix and varying amounts of yttrium (0.1-0.5 wt.%) as reinforcement are developed through cold compaction. The microstructures of the developed composite samples revealed that the yttrium reinforcement caused grain refinement up to 0.3 wt.% and beyond which the refinement is not effective. The microstructure revealed Al2Cu precipitation which strengthened the composite up to 0.3 wt.% yttrium reinforcement. Upon further increase in yttrium reinforcement, the intermetallics and the precipitation coarsen and their corresponding strengthening effect decreases. The mechanical characterization revealed that the composite sample reinforced with 0.3 wt.% yttrium showed highest mechanical properties like 82 HV of hardness, 276 MPa Ultimate Tensile Strength (UTS), 229 MPa Yield Strength (YS) and an elongation (EL) of 18.9% respectively. However, the relative density of the developed composites decreased with the increase in yttrium reinforcement.
Abstract: Chip formation characteristics are investigated during surface finishing of high density polyethylene (HDPE) samples using a shaper machine. Both the cutting speed and depth of cut are varied continually to enable observations under various machining conditions. The generated chips are analyzed in terms of their shape, size, and deformation. Their physical appearances are also observed using digital camera and optical microscope. The investigation shows that continuous chips are obtained for all the cutting conditions. It is observed that cutting speed is more influential than depth of cut to cause dimensional changes of chips. Chips curl radius is also found to increase gradually with the increase of cutting speed. The length of continuous chips remains always smaller than the job length, and the corresponding discrepancies are found to be more prominent at lower cutting speed. Microstructures of the chips reveal that cracks are formed at higher cutting speeds and depth of cuts, which is not that significant at low depth of cut.
Abstract: CoNiCrAlY alloys have been widely used as bond coats for thermal barrier coating (TBC) systems because of low cost, improved control of composition, and the feasibility to tailor the coatings microstructures. Coatings are in general very thin structures, and therefore it is impossible to characterize the mechanical responses of the materials via conventional mechanical testing methods. Due to this reason, miniature specimen testing methods, such as the small punch test technique, have been developed. This paper presents some of the recent research in evaluating the mechanical properties of the CoNiCrAlY coatings at room and high temperatures, through the use of small punch testing and the developed miniature specimen tensile testing, applicable to a range of temperature, to investigate the elastic-plastic and creep behavior as well as ductile-brittle transition temperature (DBTT) behavior. An inverse procedure was developed to derive the mechanical properties from such tests for the coating materials. A two-layer specimen test method is also described. The key findings include: 1) the temperature-dependent coating properties can be accurately determined by the miniature tensile testing within a wide range of temperature; 2) consistent DBTTs can be identified by both the SPT and miniature tensile tests (~ 650 °C); and 3) the FE SPT modelling has shown good capability of simulating the early local cracking. In general, the temperature-dependent material behaviors of the CoNiCrAlY coating has been effectively characterized using miniature specimen testing and inverse method.
Abstract: The hardness-microstructure relationships of spherical cementite in bainitic matrix obtained by a different heat treatment cycles carried out to high carbon powder metallurgy (P/M) steel were investigated. For this purpose, 1.5 wt.% natural graphite powder admixed in atomized iron powders and the mixed powders were compacted under 700 MPa at room temperature and then sintered at 1150 °C under a protective argon gas atmosphere. The densities of the green and sintered samples were measured via the Archimedes method. A density of 7.4 g/cm3 was obtained after sintering and a density of 94% was achieved. The sintered specimens having primary cementite plus lamellar pearlitic structures were fully quenched from 950 °C temperature and then over-tempered at 705 °C temperature for 60 minutes to produce spherical-fine cementite particles in the ferritic matrix. After by this treatment, these samples annealed at 735 °C temperature for 3 minutes were austempered at 300 °C salt bath for a period of 1 to 5 hours. As a result of this process, it could be able to produced spherical cementite particle in the bainitic matrix. This microstructure was designed to improve wear and toughness of P/M steels. The microstructures were characterized and analyzed by SEM and micro and macro hardness.
Abstract: Sheet Molding Compounds (SMCs) with special microstructures are very attractive to use in automobile structures especially when they are accidentally subjected to collision type accidents because of their high energy absorption capacity. These are materials designated as standard SMC, Advanced Sheet Molding Compounds (A-SMC), Low-Density SMC (LD-SMC) and etc. In this study, testing methods have been performed to compare the mechanical responses and damage phenomena of SMC, LD-SMC, and A-SMC under quasi-static and high strain rate tensile tests. The paper also aims at investigating the effect of an initial pre-damage induced by fatigue on the tensile dynamic behavior of A-SMC. In the case of SMCs and A-SMCs, whatever the fibers orientation and applied strain rate are, the first observed phenomenon of damage corresponds to decohesion of the fiber-matrix interface which is followed by coalescence and multiplication of these micro-cracks and their propagations. For LD-SMCs, damage mechanisms depend on the presence of Hollow Glass Microspheres (HGM) and fibers orientation.
Abstract: In this study, characteristics of ATIG welds using ZnO flux on aluminum was investigated and compared with TIG welds. Autogenously AC-ATIG bead on plate welding was applied on Al1050 plate with a coating of ZnO as the flux. Different levels of welding current and flux layer thickness was considered to study the effect of heat input and flux quantity on ATIG welds and was compared with those of TIG welds. Geometrical investigation of the weld cross sections revealed that penetration depth of the ATIG welds with ZnO flux, was increased up to 2 times in some samples compared to the TIG welds. Optical metallographic and Scanning Electron Microscopy (SEM) observations revealed similar microstructures in TIG and ATIG welds. Composition of the ATIG welds slag was also analyzed using X-ray diffraction. In both TIG and ATIG samples, the lowest values of microhardness were observed in the HAZ.
Abstract: This study focuses on the effect of the addition of magnesium (Mg) and silver (Ag) on the mechanical properties of aluminum based alloys. The alloying elements will be added at different levels using the factorial design of experiments of 22; the two factors are Mg and Ag at two levels of concentration. The superior mechanical properties of the produced Al-Cu-Mg-Ag alloys after aging will be resulted from a unique type of precipitation named as Ω-phase. The formed precipitate enhanced the tensile strength and thermal stability. This paper further investigated the microstructure and mechanical properties of as cast Al–Cu–Mg–Ag alloys after being complete homogenized treatment at 520 °C for 8 hours followed by isothermally age hardening process at 190 °C for different periods of time. The homogenization at 520 °C for 8 hours was selected based on homogenization study at various temperatures and times. The alloys’ microstructures were studied by using optical microscopy (OM). In addition to that, the fracture surface investigation was performed using a scanning electronic microscope (SEM). Studying the microstructure of aged Al-Cu-Mg-Ag alloys reveal that the grains are equiaxed with an average grain size of about 50 µm. A detailed fractography study for fractured surface of the aged alloys exhibited a mixed fracture whereby the random fracture suggested crack propagation along the grain boundaries while the dimples indicated that the fracture was ductile. The present result has shown that alloy 5 has the highest hardness values and the best mechanical behaviors.
Abstract: Nowadays construction industry is developing means to incorporate waste products in concrete to ensure sustainability. To meet the need of construction industry, a synthetic aggregate was developed using optimized technique called compression moulding press technique. The manufactured aggregate comprises mixture of plastic, waste which acts as binder, together with by-product waste which acts as fillers. The physical properties and microstructures of the inert materials and the manufactured aggregate were examined and compared with the conventional available aggregates. The outcomes suggest that the developed aggregate has potential to be used as substitution of conventional aggregate due to its less weight and water absorption. The microstructure analysis confirmed the efficiency of the manufacturing process where the final product has the same mixture of binder and filler.
Abstract: Fe-based amorphous feedstock powders are used as the matrix into which various ratios of hard B4C nanoparticles (0, 5, 10, 15, 20 vol.%) as reinforcing agents were prepared using a planetary high-energy mechanical milling. The ball-milled nanocomposite feedstock powders were also sprayed by means of high-velocity oxygen fuel (HVOF) technique. The characteristics of the powder particles and the prepared coating depending on their microstructures and nanohardness were examined in detail using nanoindentation tester. The results showed that the formation of the Fe-based amorphous phase was noticed over the course of high-energy ball milling. It is interesting to note that the nanocomposite coating is divided into two regions, namely, a full amorphous phase region and homogeneous dispersion of B4C nanoparticles with a scale of 10–50 nm in a residual amorphous matrix. As the B4C content increases, the nanohardness of the composite coatings increases, but the fracture toughness begins to decrease at the B4C content higher than 20 vol.%. The optimal mechanical properties are obtained with 15 vol.% B4C due to the suitable content and uniform distribution of nanoparticles. Consequently, the changes in mechanical properties of the coatings were attributed to the changes in the brittle to ductile transition by adding B4C nanoparticles.
Abstract: The present research reports the investigation of fast etching of silicon for the fabrication of microelectromechanical systems (MEMS) structures using silicon wet bulk micromachining. Low concentration tetramethyl-ammonium hydroxide (TMAH) and hydroxylamine (NH2OH) are used as main etchant and additive, respectively. The concentration of NH2OH is varied to optimize the composition to achieve best etching characteristics such as high etch rate, significantly high undercutting at convex corner for the fast release of the microstructures from the substrate, and improved etched surface morphology. These etching characteristics are studied on Si{100} and Si{110} wafers as they are most widely used in the fabrication of MEMS structures as wells diode, transistors and integrated circuits.
Abstract: Thermo-mechanical processing with various processing parameters was applied to 0.2%C-0.6%Mn-2S%i-0.8%Cr low alloyed high strength steel. The aim of the processing was to achieve the microstructures typical for transformation induced plasticity (TRIP) steels. Thermo-mechanical processing used in this work incorporated two or three deformation steps. The deformations were in all the cases carried out during the cooling from soaking temperatures to various bainite hold temperatures. In this way, 4-10% of retained austenite were retained in the final microstructures, consisting further of ferrite, bainite, martensite and pearlite. The complex character of TRIP steel microstructure is responsible for its good strength and ductility. The strengths achieved in this work were in the range of 740 MPa – 836 MPa with ductility A5mm of 31-41%.
Abstract: A high quality crack-free film of Bi2Te3 material has been deposited for the first time using electrophoretic deposition (EPD) and microstructures of various films have been investigated. One of the most important thermoelectric (TE) applications is Bi2Te3 to manufacture TE generators (TEG) which can convert waste heat into electricity targeting the global warming issue. However, the high cost of the manufacturing process of TEGs keeps them expensive and out of reach for commercialization. Therefore, utilizing EPD as a simple and cost-effective method will open new opportunities for TEG’s commercialization. This method has been recently used for advanced materials such as microelectronics and has attracted a lot of attention from both scientists and industry. In this study, the effect of media of suspensions has been investigated on the quality of the deposited films as well as their microstructure. In summary, finding an appropriate suspension is a critical step for a successful EPD process and has an important effect on both the film’s quality and its future properties.
Abstract: Electrophoretic deposition (EPD) of p-type Bi2Te3 material has been accomplished, and a high quality crack-free thick film has been achieved for thermoelectric (TE) applications. TE generators (TEG) can convert waste heat into electricity, which can potentially solve global warming problems. However, TEG is expensive due to the high cost of materials, as well as the complex and expensive manufacturing process. EPD is a simple and cost-effective method which has been used recently for advanced applications. In EPD, when a DC electric field is applied to the charged powder particles suspended in a suspension, they are attracted and deposited on the substrate with the opposite charge. In this study, it has been shown that it is possible to prepare a TE film using the EPD method and potentially achieve high TE properties at low cost. The relationship between the deposition weight and the EPD-related process parameters, such as applied voltage and time, has been investigated and a linear dependence has been observed, which is in good agreement with the theoretical principles of EPD. A stable EPD suspension of p-type Bi2Te3 was prepared in a mixture of acetone-ethanol with triethanolamine as a stabilizer. To achieve a high quality homogenous film on a copper substrate, the optimum voltage and time of the EPD process was investigated. The morphology and microstructures of the green deposited films have been investigated using a scanning electron microscope (SEM). The green Bi2Te3 films have shown good adhesion to the substrate. In summary, this study has shown that not only EPD of p-type Bi2Te3 material is possible, but its thick film is of high quality for TE applications.
Abstract: Corrosion problem which exists in every stage of oil and gas production has been a great challenge to the operators in the industry. The conventional carbon steel with all its inherent advantages has been adjudged susceptible to the aggressive corrosion environment of oilfield. This has aroused increased interest in the use of micro alloyed steels for oil and gas production and transportation. The corrosion behavior of three commercially supplied micro alloyed steels designated as A, B, and C have been investigated with API 5L X65 as reference samples. Electrochemical corrosion tests were conducted in an unbuffered 3.5 wt% NaCl solution saturated with CO2 at 30 0C for 24 hours. Pre-corrosion analyses revealed that samples A, B and X65 consist of ferrite-pearlite microstructures but with different grain sizes, shapes and distribution whereas sample C has bainitic microstructure with dispersed acicular ferrites. The results of the electrochemical corrosion tests showed that within the experimental conditions, the corrosion rate of the samples can be ranked as CR(A)< CR(X65)< CR(B)< CR(C). These results are attributed to difference in microstructures of the samples as depicted by ASTM grain size number in accordance with ASTM E112-12 Standard and ferrite-pearlite volume fractions determined by ImageJ Fiji grain size analysis software.
Abstract: Perovskite-type membrane Ba0.5Sr0.5Ce0.9Y0.1O3-δ (BSCY) was successfully synthesized by liquid citrate method. The hydrogen permeation and stability of BSCY perovskite-type membranes were studied at high temperatures. The phase structure of the powder was characterized by X-ray diffraction (XRD). Scanning electron microscopy (SEM) was used to characterize microstructures of the membrane sintered under various conditions. SEM results showed that increasing in sintering temperature, formed dense membrane with clear grains. XRD results for BSCY membrane that sintered in 1150 °C indicated single phase perovskite structure with orthorhombic configuration, and SEM results showed dense structure with clear grain size which is suitable for permeation tests. Partial substitution of Sr with Ba in SCY structure improved the hydrogen permeation flux through the membrane due to the larger ionic radius of Ba2+. BSCY membrane shows high hydrogen permeation flux of 1.6 ml/min.cm2 at 900 °C and partial pressure of 0.6.
Abstract: Wetting efficiency of microstructures or nanostructures patterned on Si wafers is a real challenge in integrated circuits manufacturing. In fact, bad or non-uniform wetting during wet processes limits chemical reactions and can lead to non-complete etching or cleaning inside the patterns and device defectivity. This issue is more and more important with the transistors size shrinkage and concerns mainly high aspect ratio structures. Deep Trench Isolation (DTI) structures enabling pixels’ isolation in imaging devices are subject to this phenomenon. While low-frequency acoustic reflectometry principle is a well-known method for Non Destructive Test applications, we have recently shown that it is also well suited for nanostructures wetting characterization in a higher frequency range. In this paper, we present a high-frequency acoustic reflectometry characterization of DTI wetting through a confrontation of both experimental and modeling results. The acoustic method proposed is based on the evaluation of the reflection of a longitudinal acoustic wave generated by a 100 µm diameter ZnO piezoelectric transducer sputtered on the silicon wafer backside using MEMS technologies. The transducers have been fabricated to work at 5 GHz corresponding to a wavelength of 1.7 µm in silicon. The DTI studied structures, manufactured on the wafer frontside, are crossing trenches of 200 nm wide and 4 µm deep (aspect ratio of 20) etched into a Si wafer frontside. In that case, the acoustic signal reflection occurs at the bottom and at the top of the DTI enabling its characterization by monitoring the electrical reflection coefficient of the transducer. A Finite Difference Time Domain (FDTD) model has been developed to predict the behavior of the emitted wave. The model shows that the separation of the reflected echoes (top and bottom of the DTI) from different acoustic modes is possible at 5 Ghz. A good correspondence between experimental and theoretical signals is observed. The model enables the identification of the different acoustic modes. The evaluation of DTI wetting is then performed by focusing on the first reflected echo obtained through the reflection at Si bottom interface, where wetting efficiency is crucial. The reflection coefficient is measured with different water / ethanol mixtures (tunable surface tension) deposited on the wafer frontside. Two cases are studied: with and without PFTS hydrophobic treatment. In the untreated surface case, acoustic reflection coefficient values with water show that liquid imbibition is partial. In the treated surface case, the acoustic reflection is total with water (no liquid in DTI). The impalement of the liquid occurs for a specific surface tension but it is still partial for pure ethanol. DTI bottom shape and local pattern collapse of the trenches can explain these incomplete wetting phenomena. This high-frequency acoustic method sensitivity coupled with a FDTD propagative model thus enables the local determination of the wetting state of a liquid on real structures. Partial wetting states for non-hydrophobic surfaces or low surface tension liquids are then detectable with this method.
Abstract: In this study, the butt welding of the commercial AZ31 magnesium alloy sheets have been carried out by using Tungsten Inert Gas (TIG) welding process with alternative and pulsed current. Welded samples were examined with regards to hardness and microstructure. Despite some recent developments in welding of magnesium alloys, they have some problems such as porosity, hot cracking, oxide formation and so on. Samples of the welded parts have undergone metallographic and mechanical examination. Porosities and homogeneous micron grain oxides were rarely observed. Orientations of the weld microstructure in terms of heat transfer also were rarely observed and equiaxed grain morphology was dominant grain structure as in the base metal. As results, fusion zone and few locations of the HAZ of the welded samples have shown twin’s grains. Hot cracking was not observed for any samples. Weld bead geometry of the welded samples were evaluated as normal according to welding parameters. In the results, conditions of alternative and pulsed current and the samples were compared to each other with regards to microstructure and hardness.