Search results for: high-entropy ceramics

Authors: Abid Hussain, Binay Kumar

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Environment-friendly lead-free Na₀.₅₂K₀.₄₄Li₀.₀₄Nb₀.₈₄Ta₀.₁₀Sb₀.₀₆O₃ (NKLNTS) ceramic was synthesized by solid-state reaction method in search of a potential candidate to replace lead-based ceramics such as PbZrO₃-PbTiO₃ (PZT), Pb(Mg₁/₃Nb₂/₃)O₃-PbTiO₃ (PMN-PT) etc., for various applications. The ceramic was calcined at temperature 850 ᵒC and sintered at 1090 ᵒC. The powder X-Ray Diffraction (XRD) pattern revealed the formation of pure perovskite phase having tetragonal symmetry with space group P4mm of the synthesized ceramic. The surface morphology of the ceramic was studied using Field Emission Scanning Electron Microscopy (FESEM) technique. The well-defined grains with homogeneous microstructure were observed. The average grain size was found to be ~ 0.6 µm. A very large value of piezoelectric charge coefficient (d₃₃ ~ 754 pm/V) was obtained for the synthesized ceramic which indicated its potential for use in transducers and actuators. In dielectric measurements, a high value of ferroelectric to paraelectric phase transition temperature (Tm~305 ᵒC), a high value of maximum dielectric permittivity ~ 2110 (at 1 kHz) and a very small value of dielectric loss ( < 0.6) were obtained which suggested the utility of NKLNTS ceramic in high-temperature ferroelectric devices. Also, the degree of diffuseness (γ) was found to be 1.61 which confirmed a relaxor ferroelectric behavior in NKLNTS ceramic. P-E hysteresis loop was traced and the value of spontaneous polarization was found to be ~11μC/cm² at room temperature. The pyroelectric coefficient was obtained to be very high (p ∼ 1870 μCm⁻² ᵒC⁻¹) for the present case indicating its applicability in pyroelectric detector applications including fire and burglar alarms, infrared imaging, etc. NKLNTS ceramic showed fatigue free behavior over 107 switching cycles. Remanent hysteresis task was performed to determine the true-remanent (or intrinsic) polarization of NKLNTS ceramic by eliminating non-switchable components which showed that a major portion (83.10 %) of the remanent polarization (Pr) is switchable in the sample which makes NKLNTS ceramic a suitable material for memory switching devices applications. Time-Dependent Compensated (TDC) hysteresis task was carried out which revealed resistive leakage free nature of the ceramic. The performance of NKLNTS ceramic was found to be superior to many lead based piezoceramics and hence can effectively replace them for use in piezoelectric, pyroelectric and long duration ferroelectric applications.

Keywords: dielectric properties, ferroelectric properties , lead free ceramic, piezoelectric property, solid state reaction, true-remanent polarization

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Authors: Ali Kadir, O. Anwar Beg

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Thermal barrier coatings are among the most popular methods for providing corrosion protection in high temperature applications including aircraft engine systems, external spacecraft structures, rocket chambers etc. Many different materials are available for such coatings, of which ceramics generally perform the best. Motivated by these applications, the current investigation presents detailed finite element simulations of coating stress analysis for a 3- dimensional, 3-layered model of a test sample representing a typical gas turbine component scenario. Structural steel is selected for the main inner layer, Titanium (Ti) alloy for the middle layer and Silicon Carbide (SiC) for the outermost layer. The model dimensions are 20 mm (width), 10 mm (height) and three 1mm deep layers. ANSYS software is employed to conduct three types of analysis- static structural, thermal stress analysis and also computational fluid dynamic erosion/corrosion analysis (via ANSYS FLUENT). The specified geometry which corresponds to corrosion test samples exactly is discretized using a body-sizing meshing approach, comprising mainly of tetrahedron cells. Refinements were concentrated at the connection points between the layers to shift the focus towards the static effects dissipated between them. A detailed grid independence study is conducted to confirm the accuracy of the selected mesh densities. To recreate gas turbine scenarios; in the stress analysis simulations, static loading and thermal environment conditions of up to 1000 N and 1000 degrees Kelvin are imposed. The default solver was used to set the controls for the simulation with the fixed support being set as one side of the model while subjecting the opposite side to a tabular force of 500 and 1000 Newtons. Equivalent elastic strain, total deformation, equivalent stress and strain energy were computed for all cases. Each analysis was duplicated twice to remove one of the layers each time, to allow testing of the static and thermal effects with each of the coatings. ANSYS FLUENT simulation was conducted to study the effect of corrosion on the model under similar thermal conditions. The momentum and energy equations were solved and the viscous heating option was applied to represent improved thermal physics of heat transfer between the layers of the structures. A Discrete Phase Model (DPM) in ANSYS FLUENT was employed which allows for the injection of continuous uniform air particles onto the model, thereby enabling an option for calculating the corrosion factor caused by hot air injection (particles prescribed 5 m/s velocity and 1273.15 K). Extensive visualization of results is provided. The simulations reveal interesting features associated with coating response to realistic gas turbine loading conditions including significantly different stress concentrations with different coatings.

Keywords: thermal coating, corrosion, ANSYS FEA, CFD

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Authors: Alexander Harrison Greer, Edward King, Elijah Lee, Safa Obuz, Ruhao Sun, Aditya Sardesai, Toby Ma, Daniel Chow, Bryce Broadus, Calvin Costner, Troy Barnes, Biagio DeSimone, Yeshwin Sankuratri, Yiheng Chen, Holly Golecki

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Although a relatively new field, soft robotics is experiencing a rise in applicability in the secondary school setting through The Soft Robotics Toolkit, shared fabrication resources and a design competition. Exposing students outside of university research groups to this rapidly growing field allows for development of the soft robotics industry in new and imaginative ways. Soft robotic actuators have remained difficult to implement in classrooms because of their relative cost or difficulty of fabrication. Traditionally, a two-part molding system is used; however, this configuration often results in delamination. In an effort to make soft robotics more accessible to young students, we aim to develop a simple, single-mold method of fabricating soft robotic actuators from common household materials. These actuators are made by embedding a soluble polymer insert into silicone. These inserts can be made from hand-cut polystyrene, 3D-printed polyvinyl alcohol (PVA) or acrylonitrile butadiene styrene (ABS), or molded sugar. The insert is then dissolved using an appropriate solvent such as water or acetone, leaving behind a negative form which can be pneumatically actuated. The resulting actuators are seamless, eliminating the instability of adhering multiple layers together. The benefit of this approach is twofold: it simplifies the process of creating a soft robotic actuator, and in turn, increases its effectiveness and durability. To quantify the increased durability of the single-mold actuator, it was tested against the traditional two-part mold. The single-mold actuator could withstand actuation at 20psi for 20 times the duration when compared to the traditional method. The ease of fabrication of these actuators makes them more accessible to hobbyists and students in classrooms. After developing these actuators, they were applied, in collaboration with a ceramics teacher at our school, to a glove used to transfer nuanced hand motions used to throw pottery from an expert artist to a novice. We quantified the improvement in the users’ pottery-making skill when wearing the glove using image analysis software. The seamless actuators proved to be robust in this dynamic environment. Seamless soft robotic actuators created by high school students show the applicability of the Soft Robotics Toolkit for secondary STEM education and outreach. Making students aware of what is possible through projects like this will inspire the next generation of innovators in materials science and robotics.

Keywords: pneumatic actuator fabrication, soft robotic glove, soluble polymers, STEM outreach

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Authors: Nino Sulava, Brian Gilmour, Nana Rezesidze, Tamar Beridze, Rusudan Chagelishvili

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Studies of ancient metallurgy are a subject of worldwide current interest. Georgia with its famous early metalworking traditions is one of the central parts of in the Caucasus region. The aim of the present study is to introduce the results of archaeometallurgical investigations being undertaken in the mountain region of Colchis, Lechkhumi (the Tsageri Municipality of western Georgia) and establish their place in the existing archaeological context. Lechkhumi (one of the historic provinces of Georgia known from Georgian, Greek, Byzantine and Armenian written sources as Lechkhumi/Skvimnia/Takveri) is the part of the Colchian mountain area. It is one of the important but little known centres of prehistoric metallurgy in the Caucasian region and of Colchian Bronze Age culture. Reconnaissance archaeological expeditions (2011-2015) revealed significant prehistoric metallurgical sites in Lechkhumi. Sites located in the vicinity of Dogurashi Village (Tsageri Municipality) have become the target area for archaeological excavations. During archaeological excavations conducted in 2016-2018 two archaeometallurgical sites – Dogurashi I and Dogurashi II were investigated. As a result of an interdisciplinary (archaeological, geological and geophysical) survey, it has been established that at both prehistoric Dogurashi mountain sites, it was copper that was being smelted and the ore sources are likely to be of local origin. Radiocarbon dating results confirm they were operating between about the 13th and 9th century BC. More recently another similar site has been identified in this area (Dogurashi III), and this is about to undergo detailed investigation. Other prehistoric metallurgical sites are being located and investigated in the Lechkhumi region as well as chance archaeological finds (often in hoards) – copper ingots, metallurgical production debris, slag, fragments of crucibles, tuyeres (air delivery pipes), furnace wall fragments and other related waste debris. Other chance finds being investigated are the many copper, bronze and (some) iron artefacts that have been found over many years. These include copper ingots, copper, bronze and iron artefacts such as tools, jewelry, and decorative items. These show the important but little known or understood the role of Lechkhumi in the late Bronze Age culture of Colchis. It would seem that mining and metallurgical manufacture form part of the local agricultural yearly lifecycle. Colchian ceramics have been found and also evidence for artefact production, small stone mould fragments and encrusted material from the casting of a fylfot (swastika) form of Colchian bronze buckle found in the vicinities of the early settlements of Tskheta and Dekhviri. Excavation and investigation of previously unknown archaeometallurgical sites in Lechkhumi will contribute significantly to the knowledge and understanding of prehistoric Colchian metallurgy in western Georgia (Adjara, Guria, Samegrelo, and Svaneti) and will reveal the importance of this region in the study of ancient metallurgy in Georgia and the Caucasus. Acknowledgment: This work has been supported by the Shota Rustaveli National Science Foundation (grant FR # 217128).

Keywords: archaeometallurgy, Colchis, copper, Lechkhumi

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Authors: Glauco M. M. M. Lustosa, João Paulo C. Costa, Leinig Antônio Perazolli, Maria Aparecida Zaghete

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SnO2 has electrical conductivity due to the excess of electrons and structural defects, being its electrical behavior highly dependent on sintering temperature and chemical composition. The addition of metals modifiers into the crystalline structure can improve and controlling the behavior of some semiconductor oxides that can therefore develop different applications such as varistors (ceramic with non-ohmic behavior between current and voltage, i.e. conductive during normal operation and resistive during overvoltage). The polymeric precursor method, based on the complexation reaction between metal ion and policarboxylic acid and then polymerized with ethylene glycol, was used to obtain nanopowders ceramic. The metal immobilization reduces its segregation during the decomposition of the polyester resulting in a crystalline oxide with high chemical homogeneity. The preparation of films from ceramics nanoparticles using electrophoretic deposition method (EPD) brings prospects for a new generation of smaller size devices with easy integration technology. EPD allows to control time and current and therefore it can have control of the thickness, surface roughness and the film density, quickly and with low production costs. The sintering process is key to control size and grain boundary density of the film. In this step, there is the diffusion of metals that promote densification and control of intrinsic defects or change these defects which will form and modify the potential barrier in the grain boundary. The use of microwave oven for sintering is an advantageous process due to the fast and homogeneous heating rate, promoting the diffusion and densification without irregular grain growth. This research was done a comparative study of sintering temperature by use of zinc as modifier agent to verify the influence on sintering step aiming to promote densification and grain growth, which influences the potential barrier formation and then changed the electrical behavior. SnO2-nanoparticles were obtained with 1 %mol of ZnO + 0.05 %mol of Nb2O5 (SZN), deposited as film through EPD (voltage 2 kV, time of 10 min) on Si/Pt substrate. Sintering was made in a microwave oven at 800, 900 and 1000 °C. For complete coverage of the substrate by nanoparticles with low surface roughness and uniform thickness was added 0.02 g of solid iodine in alcoholic suspension SnO2 to increase particle surface charge. They were also used magneto in EPD system that improved the deposition rate forming a compact film. Using a scanning electron microscope of high resolution (SEM_FEG) it was observed nanoparticles with average size between 10-20 nm, after sintering the average size was 150 to 200 nm and thickness of 5 µm. Also, it was verified that the temperature at 1000 °C was the most efficient in sintering. The best sintering time was also recorded and determined as 40 minutes. After sintering, the films were recovered with Cr3+ ions layer by EPD, then the films were again thermally treated. The electrical characterizations (nonlinear coefficient of 11.4, voltage rupture of ~60 V and leakage current = 4.8x10−6 A), allow considering the new methodology suitable for prepare SnO2-based varistor applied for development of electrical protection devices for low voltage.

Keywords: chemical synthesis, electrophoretic deposition, microwave sintering, tin dioxide

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Authors: Sugandha Gupta, Arun Kumar Jha

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A large number of ferroelectric materials have been intensely investigated for applications in non-volatile ferroelectric random access memories (FeRAMs), piezoelectric transducers, actuators, pyroelectric sensors, high dielectric constant capacitors, etc. Bismuth layered ferroelectric materials such as Strontium Bismuth Tantalate (SBT) has attracted a lot of attention due to low leakage current, high remnant polarization and high fatigue endurance up to 1012 switching cycles. However, pure SBT suffers from various major limitations such as high dielectric loss, low remnant polarization values, high processing temperature, bismuth volatilization, etc. Significant efforts have been made to improve the dielectric and ferroelectric properties of this compound. Firstly, it has been reported that electrical properties vary with the Sr/ Bi content ratio in the SrBi2Ta2O9 compsition i.e. non-stoichiometric compositions with Sr-deficient / Bi excess content have higher remnant polarization values than stoichiometic SBT compositions. With the objective to improve structural, dielectric, ferroelectric and piezoelectric properties of SBT compound, rare earth holmium (Ho3+) was chosen as a donor cation for substitution onto the Bi2O2 layer. Moreover, hardly any report on holmium substitution in stoichiometric SrBi2Ta2O9 and non-stoichiometric Sr0.8Bi2.2Ta2O9 compositions were available in the literature. The holmium substituted SrBi2-xHoxTa2O9 (x= 0.00-2.0) and Sr0.8Bi2.2Ta2O9 (x=0.0 and 0.01) compositions were synthesized by the solid state reaction method. The synthesized specimens were characterized for their structural and electrical properties. X-ray diffractograms reveal single phase layered perovskite structure formation for holmium content in stoichiometric SBT samples up to x ≤ 0.1. The granular morphology of the samples was investigated using scanning electron microscope (Hitachi, S-3700 N). The dielectric measurements were carried out using a precision LCR meter (Agilent 4284A) operating at oscillation amplitude of 1V. The variation of dielectric constant with temperature shows that the Curie temperature (Tc) decreases on increasing the holmium content. The specimen with x=2.0 i.e. the bismuth free specimen, has very low dielectric constant and does not show any appreciable variation with temperature. The dielectric loss reduces significantly with holmium substitution. The polarization–electric field (P–E) hysteresis loops were recorded using a P–E loop tracer based on Sawyer–Tower circuit. It is observed that the ferroelectric property improve with Ho substitution. Holmium substituted specimen exhibits enhanced value of remnant polarization (Pr= 9.22 μC/cm²) as compared to holmium free specimen (Pr= 2.55 μC/cm²). Piezoelectric co-efficient (d33 values) was measured using a piezo meter system (Piezo Test PM300). It is observed that holmium substitution enhances piezoelectric coefficient. Further, the optimized holmium content (x=0.01) in stoichiometric SrBi2-xHoxTa2O9 composition has been substituted in non-stoichiometric Sr0.8Bi2.2Ta2O9 composition to obtain further enhanced structural and electrical characteristics. It is expected that a new class of ferroelectric materials i.e. Rare Earth Layered Structured Ferroelectrics (RLSF) derived from Bismuth Layered Structured Ferroelectrics (BLSF) will generate which can be used to replace static (SRAM) and dynamic (DRAM) random access memories with ferroelectric random access memories (FeRAMS).

Keywords: dielectrics, ferroelectrics, piezoelectrics, strontium bismuth tantalate

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Authors: Alberto Fina, Samuele Colonna, Maria del Mar Bernal, Orietta Monticelli, Mauro Tortello, Renato Gonnelli, Julio Gomez, Chiara Novara, Guido Saracco

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Thermally conductive polymer nanocomposites are of high interest for several applications including low-temperature heat recovery, heat exchangers in a corrosive environment and heat management in electronics and flexible electronics. In this paper, the preparation of thermally conductive nanocomposites exploiting graphene-related materials is addressed, along with their thermal characterization. In particular, correlations between 1- chemical and physical features of the nanoflakes and 2- processing conditions with the heat conduction properties of nanocomposites is studied. Polymers are heat insulators; therefore, the inclusion of conductive particles is the typical solution to obtain a sufficient thermal conductivity. In addition to traditional microparticles such as graphite and ceramics, several nanoparticles have been proposed, including carbon nanotubes and graphene, for the use in polymer nanocomposites. Indeed, thermal conductivities for both carbon nanotubes and graphenes were reported in the wide range of about 1500 to 6000 W/mK, despite such property may decrease dramatically as a function of the size, number of layers, the density of topological defects, re-hybridization defects as well as on the presence of impurities. Different synthetic techniques have been developed, including mechanical cleavage of graphite, epitaxial growth on SiC, chemical vapor deposition, and liquid phase exfoliation. However, the industrial scale-up of graphene, defined as an individual, single-atom-thick sheet of hexagonally arranged sp2-bonded carbons still remains very challenging. For large scale bulk applications in polymer nanocomposites, some graphene-related materials such as multilayer graphenes (MLG), reduced graphene oxide (rGO) or graphite nanoplatelets (GNP) are currently the most interesting graphene-based materials. In this paper, different types of graphene-related materials were characterized for their chemical/physical as well as for thermal properties of individual flakes. Two selected rGOs were annealed at 1700°C in vacuum for 1 h to reduce defectiveness of the carbon structure. Thermal conductivity increase of individual GNP with annealing was assessed via scanning thermal microscopy. Graphene nano papers were prepared from both conventional RGO and annealed RGO flakes. Characterization of the nanopapers evidenced a five-fold increase in the thermal diffusivity on the nano paper plane for annealed nanoflakes, compared to pristine ones, demonstrating the importance of structural defectiveness reduction to maximize the heat dissipation performance. Both pristine and annealed RGO were used to prepare polymer nanocomposites, by melt reactive extrusion. Thermal conductivity showed two- to three-fold increase in the thermal conductivity of the nanocomposite was observed for high temperature treated RGO compared to untreated RGO, evidencing the importance of using low defectivity nanoflakes. Furthermore, the study of different processing paremeters (time, temperature, shear rate) during the preparation of poly (butylene terephthalate) nanocomposites evidenced a clear correlation with the dispersion and fragmentation of the GNP nanoflakes; which in turn affected the thermal conductivity performance. Thermal conductivity of about 1.7 W/mK, i.e. one order of magnitude higher than for pristine polymer, was obtained with 10%wt of annealed GNPs, which is in line with state of the art nanocomposites prepared by more complex and less upscalable in situ polymerization processes.

Keywords: graphene, graphene-related materials, scanning thermal microscopy, thermally conductive polymer nanocomposites

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Authors: Glauco M. M. M. Lustosa, João Paulo C. Costa, Sonia M. Zanetti, Mario Cilense, Leinig Antônio Perazolli, Maria Aparecida Zaghete

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The contamination of the environment has been one of the biggest problems of our time, mostly due to developments of many industries. SnO2 is an n-type semiconductor with band gap about 3.5 eV and has its electrical conductivity dependent of type and amount of modifiers agents added into matrix ceramic during synthesis process, allowing applications as sensing of gaseous pollutants on ambient. The chemical synthesis by polymeric precursor method consists in a complexation reaction between tin ion and citric acid at 90 °C/2 hours and subsequently addition of ethyleneglycol for polymerization at 130 °C/2 hours. It also prepared polymeric resin of zinc, cobalt and niobium ions. Stoichiometric amounts of the solutions were mixed to obtain the systems (Zn, Nb)-SnO2 and (Co, Nb) SnO2 . The metal immobilization reduces its segregation during the calcination resulting in a crystalline oxide with high chemical homogeneity. The resin was pre-calcined at 300 °C/1 hour, milled in Atritor Mill at 500 rpm/1 hour, and then calcined at 600 °C/2 hours. X-Ray Diffraction (XDR) indicated formation of SnO2 -rutile phase (JCPDS card nº 41-1445). The characterization by Scanning Electron Microscope of High Resolution showed spherical ceramic powder nanostructured with 10-20 nm of diameter. 20 mg of SnO2 -based powder was kept in 20 ml of isopropyl alcohol and then taken to an electrophoretic deposition (EPD) system. The EPD method allows control the thickness films through the voltage or current applied in the electrophoretic cell and by the time used for deposition of ceramics particles. This procedure obtains films in a short time with low costs, bringing prospects for a new generation of smaller size devices with easy integration technology. In this research, films were obtained in an alumina substrate with interdigital electrodes after applying 2 kV during 5 and 10 minutes in cells containing alcoholic suspension of (Zn, Nb)-SnO2 and (Co, Nb) SnO2 of powders, forming a sensing layer. The substrate has designed integrated micro hotplates that provide an instantaneous and precise temperature control capability when a voltage is applied. The films were sintered at 900 and 1000 °C in a microwave oven of 770 W, adapted by the research group itself with a temperature controller. This sintering is a fast process with homogeneous heating rate which promotes controlled growth of grain size and also the diffusion of modifiers agents, inducing the creation of intrinsic defects which will change the electrical characteristics of SnO2 -based powders. This study has successfully demonstrated a microfabricated system with an integrated micro-hotplate for detection of CO and NO2 gas at different concentrations and temperature, with self-heating SnO2 - based nanoparticles films, being suitable for both industrial process monitoring and detection of low concentrations in buildings/residences in order to safeguard human health. The results indicate the possibility for development of gas sensors devices with low power consumption for integration in portable electronic equipment with fast analysis. Acknowledgments The authors thanks to the LMA-IQ for providing the FEG-SEM images, and the financial support of this project by the Brazilian research funding agencies CNPq, FAPESP 2014/11314-9 and CEPID/CDMF- FAPESP 2013/07296-2.

Keywords: chemical synthesis, electrophoretic deposition, self-heating, gas sensor

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