Abstract: The microstructure and texture evolution of cryo rolled and annealed ductile TaHfNbZrTi refractory high entropy alloy was investigated. To obtain that, the alloy is severely cryo rolled and subsequently annealed for the recrystallization process. The cryo rolled – 90% shows the presence of very fine grains and microstructural heterogeneity. The cryo rolled samples are annealed at a temperature ranging from 800°C to 1400°C, the partial recrystallization is observed at 800°C annealed condition, and at higher annealing temperatures the complete recrystallization process is noticed. The development of ND fiber texture is observed after the annealing.
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 microstructure, texture, phase stability, and tensile properties of annealed Ta0.5Nb0.5Hf0.5ZrTi1.5 alloy have been investigated in the present research. The alloy was severely hybrid-rolled up to 93.5% thickness reduction, subsequently rolled samples subjected to an annealing treatment at 800 °C and 1000 °C temperatures for 1 h. Consequently, the rolled condition and both annealed temperatures have a body-centered cubic (BCC) structure. Furthermore, quantitative texture measurements (orientation distribution function (ODF) analysis) and microstructural examinations (analytical electron backscatter diffraction (EBSD) maps) permitted to establish a good relationship between annealing texture and microstructure and universal testing machine (UTM) utilized for obtaining the mechanical properties. Impressive room temperature tensile properties combination with the tensile strength (1380 MPa) and (24.7%) elongation is achieved for the 800 °C heat-treated condition. The evolution of the coarse microstructure featured in the case of 1000 °C annealed temperature ascribed to the influence of high thermal energy.
Abstract: In structural-health monitoring of fiber reinforced plastics (FRPs), every single inorganic fiber sensor that are integrated into the bulk material requires an electrical insulation around itself, when the surrounding reinforcing fibers are electrically conductive. This results in a more accurate data acquisition only from the sensor fiber without any electrical interventions. For this purpose, thin nano-films of aluminium oxide (Al2O3)-based electrical-insulation coatings have been fabricated around the Silicon Carbide (SiC) single fiber sensors through reactive DC magnetron sputtering technique. The sputtered coatings were amorphous in nature and the thickness of the coatings increased with an increase in the sputter time. Microstructural characterization of the coated fibers performed using scanning electron microscopy (SEM) confirmed a homogeneous circumferential coating with no detectable defects or cracks on the surface. X-ray diffraction (XRD) analyses of the as-sputtered and 2 hours annealed coatings (825 & 1125 ˚C) revealed the amorphous and crystalline phases of Al2O3 respectively. Raman spectroscopic analyses produced no characteristic bands of Al2O3, as the thickness of the films was in the nanometer (nm) range, which is too small to overcome the actual penetration depth of the laser used. In addition, the influence of the insulation coatings on the mechanical properties of the SiC sensor fibers has been analyzed.
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: Chemical doping with different elements and compounds at various amounts represents the most suitable approach to improve the superconducting properties of bismuth-based superconductors for technological applications. In this paper, the influence of partial substitution of Sr(BO2)2 for SrO on the phase formation kinetics and transport properties of (Bi,Pb)-2223 HTS has been studied for the first time. Samples with nominal composition Bi1.7Pb0.3Sr2-xCa2Cu3Oy[Sr(BO2)2]x, x=0, 0.0375, 0.075, 0.15, 0.25, were prepared by the standard solid state processing. The appropriate mixtures were calcined at 845 oC for 40 h. The resulting materials were pressed into pellets and annealed at 837 oC for 30 h in air. Superconducting properties of undoped (reference) and Sr(BO2)2-doped (Bi,Pb)-2223 compounds were investigated through X-ray diffraction (XRD), resistivity (ρ) and transport critical current density (Jc) measurements. The surface morphology changes in the prepared samples were examined by scanning electron microscope (SEM). XRD and Jc studies have shown that the low level Sr(BO2)2 doping (x=0.0375-0.075) to the Sr-site promotes the formation of high-Tc phase and leads to the enhancement of current carrying capacity in (Bi,Pb)-2223 HTS. The doped sample with x=0.0375 has the best performance compared to other prepared samples. The estimated volume fraction of (Bi,Pb)-2223 phase increases from ~25 % for reference specimen to ~70 % for x=0.0375. Moreover, strong increase in the self-field Jc value was observed for this dopant amount (Jc=340 A/cm2), compared to an undoped sample (Jc=110 A/cm2). Pronounced enhancement of superconducting properties of (Bi,Pb)-2223 superconductor can be attributed to the acceleration of high-Tc phase formation as well as the improvement of inter-grain connectivity by small amounts of Sr(BO2)2 dopant.
Abstract: Graphene has gained much attention owing to its unique optical and electrical properties. Charge carriers in graphene sheets (GS) carry out a linear dispersion relation near the Fermi energy and behave as massless Dirac fermions resulting in unusual attributes such as the quantum Hall effect and ambipolar electric field effect. It also exhibits nondispersive transport characteristics with an extremely high electron mobility (15000 cm2/(Vs)) at room temperature. Recently, several progresses have been achieved in the fabrication of single- or multilayer GS for functional device applications in the fields of optoelectronic such as field-effect transistors ultrasensitive sensors and organic photovoltaic cells. In addition to device applications, graphene also can serve as reinforcement to enhance mechanical, thermal, or electrical properties of composite materials. Electrophoretic deposition (EPD) is an attractive method for development of various coatings and films. It readily applied to any powdered solid that forms a stable suspension. The deposition parameters were controlled in various thicknesses. In this study, the graphene electrodeposition conditions were optimized. The results were obtained from SEM, Ohm resistance measuring technique and AFM characteristic tests. The minimum sheet resistance of electrodeposited reduced graphene oxide layers is achieved at conditions of 2 V in 10 s and it is annealed at 200 °C for 1 minute.
Abstract: The present work aims at contributing to the study of the complex phenomenon of wear of pin on disc contact in dry sliding friction between two material couples (bronze/steel and unsaturated polyester virgin and charged with graphite powder/steel). The work consists of the determination of the coefficient of friction, the study of the influence of the tribological parameters on this coefficient and the determination of the mass loss and the wear rate of the pin. This study is also widened to the highlighting of the influence of the addition of graphite powder on the tribological properties of the polymer constituting the pin. The experiments are carried out on a pin-disc type tribometer that we have designed and manufactured. Tests are conducted according to the standards DIN 50321 and DIN EN 50324. The discs are made of annealed XC48 steel and quenched and tempered XC48 steel. The main results are described here after. The increase of the normal load and the sliding speed causes the increase of the friction coefficient, whereas the increase of the percentage of graphite and the hardness of the disc surface contributes to its reduction. The mass loss also increases with the normal load. The influence of the normal load on the friction coefficient is more significant than that of the sliding speed. The effect of the sliding speed decreases for large speed values. The increase of the amount of graphite powder leads to a decrease of the coefficient of friction, the mass loss and the wear rate. The addition of graphite to the UP resin is beneficial; it plays the role of solid lubricant.
Abstract: The corrosion behaviour of 316L stainless steel coatings obtained by cold spray method was investigated in this study. 316L powders were deposited onto Al5052 aluminum substrates. The coatings were produced using nitrogen (N2) process gas. In order to further improve the corrosion and mechanical properties of the coatings, heat treatment was applied at 250 and 750 °C. The corrosion performances of the coatings were compared using the potentiodynamic scanning (PDS) technique under in-vitro conditions (in Ringer’s solution at 37 °C). In addition, the hardness and porosity tests were carried out on the coatings. Microstructural characterization of the coatings was carried out by using scanning electron microscopy attached with energy dispersive spectrometer (SEM-EDS) and X-ray diffraction (XRD) technique. It was found that clean surfaces and a good adhesion were achieved for particle/substrate bonding. The heat treatment process provided both elimination of the anisotropy in the coating and resulting in healing-up of the incomplete interfaces between the deposited particles. It was found that the corrosion potential of the annealed coatings at 750 °C was higher than that of commercially 316 L stainless steel. Moreover, the microstructural investigations after the corrosion tests revealed that corrosion preferentially starts at inter-splat boundaries.
Abstract: In this paper, a simple chemical precipitation route for the preparation of titanium dioxide nanoparticles, synthesized by using titanium tetra isopropoxide as a precursor and polyvinyl pyrrolidone (PVP) as a capping agent, is reported. The Differential Scanning Calorimetry (DSC) and Thermo Gravimetric Analysis (TGA) of the samples were recorded and the phase transformation temperature of titanium hydroxide, Ti(OH)4 to titanium oxide, TiO2 was investigated. The as-prepared Ti(OH)4 precipitate was annealed at 800°C to obtain TiO2 nanoparticles. The thermal, structural, morphological and textural characterizations of the TiO2 nanoparticle samples were carried out by different techniques such as DSC-TGA, X-Ray Diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Micro Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence spectroscopy (PL) and Field Effect Scanning Electron Microscopy (FESEM) techniques. The as-prepared precipitate was characterized using DSC-TGA and confirmed the mass loss of around 30%. XRD results exhibited no diffraction peaks attributable to anatase phase, for the reaction products, after the solvent removal. The results indicate that the product is purely rutile. The vibrational frequencies of two main absorption bands of prepared samples are discussed from the results of the FTIR analysis. The formation of nanosphere of diameter of the order of 10 nm, has been confirmed by FESEM. The optical band gap was found by using UV-Visible spectrum. From photoluminescence spectra, a strong emission was observed. The obtained results suggest that this method provides a simple, efficient and versatile technique for preparing TiO2 nanoparticles and it has the potential to be applied to other systems for photocatalytic activity.
Abstract: Lithium niobate (LiNbO3) nanostructures are prepared on quartz substrate by the sol-gel method. They have been deposited with different molarity concentration and annealed at 500°C. These samples are characterized and analyzed by X-ray diffraction (XRD), Scanning Electron Microscope (SEM) and Atomic Force Microscopy (AFM). The measured results showed an importance increasing in molarity concentrations that indicate the structure starts to become crystal, regular, homogeneous, well crystal distributed, which made it more suitable for optical waveguide application.
Abstract: This study attempts to understand the effect of different UV irradiation methods on the intercalation of LDPE/MMT nanocomposites, and its molecular behavior at certain isothermal crystallization temperature. Three different methods of UV exposure were employed using single composition of LDPE/MMT nanocomposites. All samples were annealed for 5 hours at a crystallization temperature of 100oC. The crystallization temperature was chosen to be at large supercooling temperature to ensure quick and complete crystallization. The raw material of LDPE consisted of two stable monoclinic and orthorhombic phases according to XRD results. The thermal behavior of both phases acted differently when UV exposure method was changed. The monoclinic phase was more dependent on the method used compared to the orthorhombic phase. The intercalation of clay, as well as, the non-isothermal crystallization temperature, has also shown a clear dependency on the type of UV exposure. A third phase that is thermally less stable was also observed. Its respond to UV irradiation was greater since it contains low molecular weight entities which make it more vulnerable to any UV exposure.
Abstract: Effect of Zn addition on the microstructure and
mechanical properties of Mg-Zn alloys with Zn contents from 6 to 10
weight percent was investigated in this study. Through calculation of
phase equilibria of Mg-Zn alloys, carried out by using FactSage® and
FTLite database, solution treatment temperature was decided as
temperatures from 300 to 400oC, where supersaturated solid solution
can be obtained. Solid solution treatment of Mg-Zn alloys was
successfully conducted at 380oC and supersaturated microstructure
with all beta phase resolved into matrix was obtained. After solution
treatment, hot rolling was successfully conducted by reduction of
60%. Compression and tension tests were carried out at room
temperature on the samples as-cast, solution treated, hot-rolled and
recrystallized after rolling. After solid solution treatment, each alloy
was annealed at temperatures of 180 and 200oC for time intervals from
1 min to 48 hrs and hardness of each condition was measured by
micro-Vickers method. Peak aging conditions were deduced as at the
temperature of 200oC for 10 hrs. By addition of Zn by 10 weight
percent, hardness and strength were enhanced.
Abstract: Microstructure and mechanical properties of AZ91D
Mg alloys for nonflammable use, containing Ca and Y, were
investigated in this study. Solid solution treatment of AZ91D Mg alloy
with Ca and Y was successfully conducted at 420oC and
supersaturated microstructure with almost all beta phases resolved into
matrix was obtained. After solid solution treatment, the alloy was
annealed at temperatures of 180 and 200oC for time intervals from 1
min to 48 hrs and hardness of each condition was measured by
micro-Vickers method. Peak aging conditions were deduced from the
results as at the temperature of 200oC for 10 hrs. Hot rolling was also
carried out at 400oC by the reduction ratio of 0.6 through 5 passes
followed by recrystallization treatment. Tensile and compressive
properties were measured at room temperature on the specimens of
each process, i.e. as-cast, solution treatment, hot rolling, and
recrystallization.
Abstract: Si ion implantation was widely used to synthesize
specimens of SiO2 containing supersaturated Si and subsequent high
temperature annealing induces the formation of embedded
luminescent Si nanocrystals. In this work, the potentialities of excimer
UV-light (172 nm, 7.2 eV) irradiation and rapid thermal annealing
(RTA) to enhance the photoluminescence and to achieve low
temperature formation of Si nanocrystals have been investigated. The
Si ions were introduced at acceleration energy of 180 keV to fluence of
7.5 x 1016 ions/cm2. The implanted samples were subsequently
irradiated with an excimer-UV lamp. After the process, the samples
were rapidly thermal annealed before furnace annealing (FA).
Photoluminescence spectra were measured at various stages at the
process. We found that the luminescence intensity is strongly
enhanced with excimer-UV irradiation and RTA. Moreover, effective
visible photoluminescence is found to be observed even after FA at
900 oC, only for specimens treated with excimer-UV lamp and RTA.
We also prepared specimens of Si nanocrystals embedded in a SiO2 by
reactive pulsed laser deposition (PLD) in an oxygen atmosphere. We
will make clear the similarities and differences with the way of
preparation.
Abstract: The nanoindentation behaviour and phase
transformation of annealed single-crystal silicon wafers are examined.
The silicon specimens are annealed at temperatures of 250, 350 and
450ºC, respectively, for 15 minutes and are then indented to maximum
loads of 30, 50 and 70 mN. The phase changes induced in the indented
specimens are observed using transmission electron microscopy
(TEM) and micro-Raman scattering spectroscopy (RSS). For all
annealing temperatures, an elbow feature is observed in the unloading
curve following indentation to a maximum load of 30 mN. Under
higher loads of 50 mN and 70 mN, respectively, the elbow feature is
replaced by a pop-out event. The elbow feature reveals a complete
amorphous phase transformation within the indented zone, whereas
the pop-out event indicates the formation of Si XII and Si III phases.
The experimental results show that the formation of these crystalline
silicon phases increases with an increasing annealing temperature and
indentation load. The hardness and Young’s modulus both decrease as
the annealing temperature and indentation load are increased.
Abstract: Microstructural and hardening changes of
Fe-0.2wt.%V alloy and pure Fe irradiated with 100 keV hydrogen ions
at room temperature were investigated. It was found that dislocation
density varies dramatically after irradiation, ranging from dislocation
free to dense areas with tangled and complex dislocation
configuration. As the irradiated Fe-0.2wt.%V samples were annealed
at 773 K, the irradiation-induced dislocation loops disappear, while
many small precipitates with enriched C distribute in the matrix. Some
large precipitates with enriched V were also observed. The hardness of
Fe-0.2wt.%V alloy and pure Fe increases after irradiation, which
ascribes to the formation of dislocation loops in the irradiated
specimens. Compared with pure Fe, the size of the
irradiation-introduced dislocation loops in Fe-0.2wt.%V alloy
decreases and the density increases, the change of the hardness also
decreases.
Abstract: A nanocrystalline thin film of ZnSe was successfully
electrodeposited on copper substrate using a non-aqueous solution
and subsequently annealed in air at 400°C. XRD analysis indicates
the polycrystalline deposit of (111) plane in both the cases. The
sharpness of the peak increases due to annealing of the film and
average grain size increases to 20 nm to 27nm. SEM photograph
indicate that grains are uniform and densely distributed over the
surface. Annealing increases the average grain size by 20%. The EDS
spectroscopy shows the ratio of Zn & Se is 1.1 in case of annealed
film. AFM analysis indicates the average roughness of the film
reduces from 181nm to 165nm due to annealing of the film. The
bandgap also decreases from 2.71eV to 2.62eV.
Abstract: In this article a comparison was made between Cu and
TiO2 supported catalysts on activated carbon for ozone
decomposition reaction. The activated carbon support in the case of
TiO2/AC sample was prepared by physicochemical pyrolysis and for
Cu/AC samples the supports are chemically modified carbons. The
prepared catalysts were synthesized by impregnation method. The
samples were annealed in two different regimes- in air and under
vacuum. To examine adsorption efficiency of the samples BET
method was used. All investigated catalysts supported on chemically
modified carbons have higher specific surface area compared to the
specific surface area of TiO2 supported catalysts, varying in the range
590÷620 m2/g. The method of synthesis of the precursors had
influenced catalytic activity.