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At least 1,297 records · Page 72

TRITIUM TRANSPORT MODELING AT THE PORE SCALE IN CERAMIC BEEDER MATERIALS USING TMAP8

Fusion reactors depend on the blanket material to breed and release tritium at the same rate or faster than it is consumed by the fusion reaction. Cellular ceramic breeders are dense materials that can maintain a high tritium breeding ratio while promoting tritium release thanks to highly connected pores. Assessing the tritium breeding capabilities of these materials requires a combination of extensive experimental and modeling efforts. In this work, we develop and calibrate a multiphysics model of tritium transport. This novel model accounts for ceramic and pore diffusion, trapping and detrapping, and several surface reactions at the pore surface. We perform a sensitivity analysis and calibrate the model by comparing its predictions against experimental measurements of deuterium absorption. The calibrated model is then used to model tritium absorption in samples with different pore microstructures to investigate the effect of pore interconnectivity on tritium absorption. The model is part of the development of the multiscale, multiphysics framework for tritium transport (i.e., the Tritium Migration Analysis Program [TMAP8]), which is itself built on top of the finite element multiphysics framework MOOSE. This study demonstrates some of TMAP8’s capabilities, and is the first step toward assessing the tritium breeding capabilities of ceramic breeder material designs.

08 HYDROGEN↗

A short note on physical properties to irradiated nuclear fuel by means of X-ray diffraction and neutron scattering techniques

For nuclear reactor applications, understanding the evolution of the fuel materials microstructure during irradiation are of great importance. This paper reviews the physical properties of irradiated nuclear fuel analysis which are considered to be of most importance in determining the performance behavior of fuel. X-rays diffraction was recognize as important tool to investigate the phase identification while neutron scattering analyses the interaction between uranium and other materials and also investigation of the defect structure.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Synthesis, thermal and electrical properties of Al-doped Bi{sub 4}V{sub 1.8}Cu{sub 0.2}O{sub 10.7}

Partial substitution of copper with aluminum in Bi{sub 4}V{sub 1.8}Cu{sub 0.2}O{sub 10.7} has led to the Bi{sub 4}V{sub 1.8}Cu{sub 0.2−x}Al{sub x}O{sub 10.7+x/2} solid solution. X-ray diffraction and thermal analysis have shown that the compounds with x=0.05 and x=0.10 are tetragonal with γ′ form of Bi{sub 4}V{sub 2}O{sub 11}, while the compound with x=0.15 is of β polymorph. The effect of Al{sup 3+} doping on electrical conductivity has been studied using Electrochemical Impedance Spectroscopy. The electrical conductivity of doped samples along with the amount of Al{sup 3+} has been studied by electrochemical impedance spectroscopy in the temperature range 250–700 °C. The slope changes observed in the Arrhenius plots agree with the microstructural transitions occurring in these compounds. The highest ionic conductivity values are obtained for the sample with x=0.05. - Graphical abstract: Arrhenius plots of the electrical conductivity of the of Bi{sub 4}V{sub 1.8}Cu{sub 0.2−x}Al{sub x}O{sub 10.7+x/2} compounds. Display Omitted.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Benchmarking machine learning strategies for phase-field problems

Abstract We present a comprehensive benchmarking framework for evaluating machine-learning approaches applied to phase-field problems. This framework focuses on four key analysis areas crucial for assessing the performance of such approaches in a systematic and structured way. Firstly, interpolation tasks are examined to identify trends in prediction accuracy and accumulation of error over simulation time. Secondly, extrapolation tasks are also evaluated according to the same metrics. Thirdly, the relationship between model performance and data requirements is investigated to understand the impact on predictions and robustness of these approaches. Finally, systematic errors are analyzed to identify specific events or inadvertent rare events triggering high errors. Quantitative metrics evaluating the local and global description of the microstructure evolution, along with other scalar metrics representative of phase-field problems, are used across these four analysis areas. This benchmarking framework provides a path to evaluate the effectiveness and limitations of machine-learning strategies applied to phase-field problems, ultimately facilitating their practical application.

36 MATERIALS SCIENCE↗

Experimental and Theoretical Thermokinetic Analysis of the Na 3 VO 4 –CO 2 Reaction System under Different Physicochemical Conditions

Sodium vanadate (Na 3 VO 4 ) was synthesized, structural and microstructurally characterized as well as tested as possible carbon dioxide (CO 2 ) captor through thermodynamic calculations in addition to thermogravimetric dynamic and isothermal analyses. Ceramic structural characterization evidenced the formation of the Na 3 VO 4 crystal phase, while microstructural features evidenced dense agglomerates with a poor specific surface area, although synthesis temperature (600 °C) was not as high as that for other sodium ceramics. Na 3 VO 4 was investigated for the CO 2 capture process through dynamic and isothermal experiments, in the presence or absence of oxygen. All these experiments showed that Na 3 VO 4 possesses interesting CO 2 capture properties in a specific temperature range (520 and 600 °C). Isothermal products characterization allowed to elucidate the reaction pathway, implying the Na 4 V 2 O 7 formation, as possible reactive intermediate. In fact, reaction path evolution was supported with theoretical thermodynamic data. Moreover, the kinetic analysis, performed using the Avrami-Erofeev mathematical model and subsequent thermodynamic data obtention, probed the positive influence of the temperature, in both CO 2 superficial and bulk chemical sorption processes, while oxygen addition did not enhance the superficial process. Additionally, as it would be expected, kinetics were enhanced as a function of the CO 2 concentration.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Franklin expedition lead exposure: New insights from high resolution confocal x-ray fluorescence imaging of skeletal microstructure

In the summer of 1845, under the command of Sir John Franklin, 128 officers and men aboard Royal Navy ships HMS Erebus and HMS Terror sailed into Lancaster Sound and entered the waters of Arctic North America. The goal of this expedition was to complete the discovery of a northwest passage by navigating the uncharted area between Barrow Strait and Simpson Strait. Franklin and his crew spent the first winter at Beechey Island, where three crewmen died and were buried. In September 1846, the ships became stranded in ice off the northwest coast of King William Island, where they remained until April 1848. At that time, the crew, reduced to 105, deserted the ships and retreated south along the island’s western and southern shores in a desperate attempt to reach the mainland and via the Back River, to obtain aid at a Hudson’s Bay Company Post. Sadly, not one individual survived. Previous analyses of bone, hair, and soft tissue samples from expedition remains found that crewmembers’ tissues contained elevated lead (Pb) levels, suggesting that Pb poisoning may have contributed to their demise; however, questions remain regarding the timing and degree of exposure and, ultimately, the extent to which the crewmembers may have been impacted. To address this historical question, we investigated three hypotheses. First, if elevated Pb exposure was experienced by the crew during the expedition, we hypothesized that those sailors who survived longer (King William Island vs. Beechey Island) would exhibit more extensive uptake of Pb in their bones and vice versa. Second, we hypothesized that Pb would be elevated in bone microstructural features forming at or near the time of death compared with older tissue. Finally, if Pb exposure played a significant role in the failure of the expedition we hypothesized that bone samples would exhibit evidence of higher and more sustained uptake of Pb than that of a contemporary comparator naval population from the 19 th century. To test these hypotheses, we analyzed bone and dental remains of crew members and compared them against samples derived from the Royal Navy cemetery in Antigua. Synchrotron-based high resolution confocal X-ray fluorescence imaging was employed to visualize Pb distribution within bone and tooth microstructures at the micro scale. The data did not support our first hypothesis as Pb distribution within the samples from the two different sites was similar. Evidence of Pb within skeletal microstructural features formed near the time of death lent support to our second hypothesis but consistent evidence of a marked elevation in Pb levels was lacking. Finally, the comparative analysis with the Antigua samples did not support the hypothesis that the Franklin sailors were exposed to an unusually high level of Pb for the time period. Taken all together our skeletal microstructural results do not support the conclusion that Pb played a pivotal role in the loss of Franklin and his crew.

59 BASIC BIOLOGICAL SCIENCES↗

Interfacial diffusion reactions and mechanical properties of Ti3Al/Ni-based superalloy joints brazed with AgCuPd filler metal

Highlights: • Ti{sub 3}Al alloy to Ni-based superalloy was successfully brazed using Ag-21Cu-25Pd filler metal. • Phases TiPd (fcc), Ti{sub 3}Pd{sub 5} (bct) and AlPd (hcp) formed within the Ti{sub 3}Al/Ni-based superalloy joint. • Diffusion behavior of elements and its influence on joint interfacial microstructure were revealed. • A formation model of interfacial microstructure has been established. • The joint tensile strength at room temperature reached 404MPa, and the strength of 212MPa was maintained at 773 K. - Abstract: Dissimilar joining of a Ti{sub 3}Al-based alloy to a Ni-based superalloy has been conducted using Ag-21Cu-25Pd filler metal. The joint microstructures were analyzed using SEM, EPMA, XRD and TEM. The reaction behaviors between different elements were discussed. Due to the strong affinity, element Pd mainly reacted with Ti{sub 3}Al substrate and formed intermetallic compounds of TiPd, Ti{sub 3}Pd{sub 5} and AlPd. Elements Ni and Ti reacted with each other and caused the formation of Ni{sub 3}Ti in the centre of the joint. Owing to the diffusion effect, element Ag was enriched in the joint central area as (Ag,Cu){sub ss}. With the prolonging of the brazing time varying from 3 min to 15 min at 1253 K, the tensile strength of the joint firstly increased and then decreased. The joints brazed at 1253 K for 10 min presented the maximum strength of 404 MPa at room temperature, and the joint strength of 212 MPa was maintained at 773 K. The total fracture surface covered the most of the reaction zones from the (Ag,Cu){sub ss} to the diffusion effect zone at the Ti{sub 3}Al side.

36 MATERIALS SCIENCE↗

The microstructure of capsule containing self-healing materials: A micro-computed tomography study

Autonomic self-healing materials are materials with built-in (micro-) capsules or vessels, which upon fracturing release healing agents in order to recover the material's physical and mechanical properties. In order to better understand and engineer these materials, a thorough characterization of the material's microstructural behavior is essential and often overlooked. In this context, micro-computed tomography (μCT) can be used to investigate the three dimensional distribution and (de)bonding of (micro-) capsules in their native state in a polymer system with self-healing properties. Furthermore, in-situ μCT experiments in a self-healing polymer and a self-healing concrete system can elucidate the breakage and leakage behavior of (micro-) capsules at the micrometer scale. While challenges related to image resolution and contrast complicate the characterization in specific cases, non-destructive 3D imaging with μCT is shown to contribute to the understanding of the link between the microstructure and the self-healing behavior of these complex materials. - Highlights: • μCT imaging allows for the analysis of microcapsule distribution patterns in self-healing materials. • μCT allows for qualitative and quantitative measurements of healing agent release from carriers in self-healing materials. • Experimental set-ups can be optimized by changing chemical compounds in the system to ensure maximum quality imaging.

36 MATERIALS SCIENCE↗

Effect of Sm-Rich Phase on Corrosion Behavior of Hot-Extruded AZ31-1.5Sm Magnesium Alloy

The effects of Sm on the corrosion and microstructure behavior of hot-extruded AZ31 magnesium alloy were investigated by SEM, TEM, weight loss analysis, and electrochemical measurements. The results indicated that granular Al{sub 2}Sm phase ~ 4 μm in size in the hot-extruded AZ31 magnesium alloy modified with 1.5 wt.% Sm leads to significant grain refinement. The corrosion rate decreased from 15.98 × 10{sup −4} to 11.19 × 10{sup −4} g cm{sup −2} h{sup −1} in the transverse section and from 8.57 × 10{sup −4} to 6.20 × 10{sup −4} g cm{sup −2} h{sup −1} in the longitudinal section. Compared to the unmodified alloy, the corrosion potential of the Sm-modified alloy in the transverse and longitudinal sections increased by 98 and 62 mV, respectively, and the R{sub ct} value (charge transfer resistance) in the transverse and longitudinal sections of the modified alloy increased from 1764 and 1756 to 2928 and 2408 Ω cm{sup 2}, respectively. The results showed that the corrosion resistance of hot-extruded AZ31 magnesium alloy was significantly improved by Sm addition due to the grain refinement, the decreased dislocation density, and the suppression of micro-galvanic corrosion caused by Al-Sm-(Mn) intermetallic compounds.

36 MATERIALS SCIENCE↗

Segmentation of tomography datasets using 3D convolutional neural networks

Dendritic microstructures are ubiquitous in nature and are the primary solidification morphologies in metallic materials. Techniques such as X-ray computed tomography (XCT) have provided new insights into dendritic phase transformation phenomena. However, manual identification of dendritic morphologies in microscopy data can be both labor intensive and potentially ambiguous. The analysis of 3D datasets is particularly challenging due to their large sizes (terabytes) and the presence of artifacts scattered within the imaged volumes. Here, in this study, we trained 3D convolutional neural networks (CNNs) to segment 3D datasets. Three CNN architectures were investigated, including a new version of FCDenseNet which we extended to 3D. We show that using hyperparameter optimization (HPO) and fine-tuning techniques, both 2D and 3D CNN architectures outperform the previous state of the art. The 3D U-Net architecture trained in this study produced the best segmentations according to quantitative metrics (intersection-over-union of 95.56% and a boundary displacement error of 0.58 pixels), while 3D FCDense produced the smoothest boundaries and best segmentations according to visual inspection. The trained 3D CNNs are able to segment entire 852 × 852 × 250 voxel 3D volumes in only ~60 s, thus hastening the progress towards a deeper understanding of phase transformation phenomena such as dendritic solidification.

36 MATERIALS SCIENCE↗

Phase structures and morphologies of tempered CA6NM stainless steel welded by hybrid laser-arc process

The post-weld tempered microstructure of hybrid laser-arc welded CA6NM, a cast low carbon martensitic stainless steel, was investigated. The microstructural evolutions from the fusion zone to the base metal were characterized in detail using optical microscopy, scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), X-ray diffraction (XRD) and microhardness techniques. The fusion zone, in its post-weld tempered condition, consisted of tempered lath martensite, residual delta-ferrite with various morphologies, reversed austenite and chromium carbides. The reversed austenite, which can be detected through both EBSD and XRD techniques, was found to be finely dispersed along the martensite lath boundaries, particularly at triple junctions. Based on the EBSD analysis, the orientation relationship between the reversed austenite and the adjacent martensite laths seemed to follow the Kurdjumov-Sachs (K-S) model. The results also revealed the presence of the reversed austenite in the different regions of the heat affected zone after post-weld tempering. The microindentation hardness distribution was measured, and correlated to the evolution of the corresponding microstructure across the welds. - Highlights: •The EBSD analysis was performed on hybrid laser-arc welded CA6NM. •The FZ consisted of tempered lath martensite, reversed austenite, carbides and δ ferrite after tempering. •The reversed γ was formed along the α′ lath boundaries, particularly at triple junctions.

36 MATERIALS SCIENCE↗

Analysis of Pitting Corrosion on Wrought and Additively Manufactured 316L Stainless Steel in Atmospheric Environments

Additive manufacturing of metal components enables rapid fabrication of complex geometries. However, metal additive manufacturing also introduces new morphological and microstructural characteristics which might be detrimental to component performance. Here we report the pitting corrosion properties of wrought and additively manufactured 316L stainless steel after atmospheric exposure to coastal environments and laboratory-created environments. Qualitative visualization in combination with quantitative analysis of resulting pits provided an in-depth understanding of pitting differences between wrought and additively manufactured 316L stainless steel and between coastal and laboratory-based exposure. Optical and scanning electron microscopy were utilized for visualization, while white light interferometry measured pits across approximately 5mm x 5mm areas on each sample. Post-processing of the interferometry data enables quantification of pitting attack for each sample in terms of both pit depth and pit volume. The pitting analysis introduced herein offers a new technique to compare pitting attack between different manufacturing processes and materials.

36 MATERIALS SCIENCE↗

Investigation of the changes in microstructure and transport properties of leached cement pastes accounting for mix composition

Ca-leaching of cement-based materials induces detrimental effects on properties related to long-term durability. A better understanding of leaching degradation in terms of alterations in mineralogy, microstructure, and transport properties is important for long-term assessments of concrete and reinforced concrete structures used in nuclear waste disposal systems or in hydro structures. However, the decalcification process is not easy to study because it is extremely slow. In this study, an ammonium nitrate (NH{sub 4}NO{sub 3}) solution of 6 mol/l was used to accelerate the leaching kinetics. The experiments were performed on cement paste samples with different water/powder (w/p) and limestone filler (LS) replacement ratios. Both the change of sample mass over time and the amount of calcium ion leached out were monitored during the test. Different post-analysis techniques including SEM/SEM-EDX, XRD/QXRD, MIP, ion chromatography, and N{sub 2}-adsorption were used to characterize the microstructural and mineralogical changes. The effect of accelerated leaching on transport properties was studied by measuring the changes in water permeability and diffusivity of dissolved gases. Results showed that the square-root-time law of degradation was applicable under accelerated conditions. Both higher w/p ratios and LS replacements increased the rate of leaching propagation; the former had a more significant effect. The accelerated leaching significantly altered the microstructure of the cement paste to a material with a higher specific surface area, increased total porosity and a shift to larger pore sizes. Those changes led to a significant increase in water permeability (one to two orders of magnitude) and diffusivity (less than one order) depending on degradation state.

36 MATERIALS SCIENCE↗

A fractional model for anomalous diffusion with increased variability: Analysis, algorithms and applications to interface problems

Fractional equations have become the model of choice in several applications where heterogeneities at the microstructure result in anomalous diffusive behavior at the macroscale. Here, we introduce a new fractional operator characterized by a doubly-variable fractional order and possibly truncated interactions. Under certain conditions on the model parameters and on the regularity of the fractional order we show that the corresponding Poisson problem is well-posed. Additionally, we introduce a finite element discretization and describe an efficient implementation of the finite-element matrix assembly in the case of piecewise constant fractional order. Through several numerical tests, we illustrate the improved descriptive power of this new operator across media interfaces. Furthermore, we present one-dimensional and two-dimensional h-convergence results that show that the variable-order model has the same convergence behavior as the constant-order model.

97 MATHEMATICS AND COMPUTING↗

Cross-plane thermal properties of transition metal dichalcogenides

In this work, we explore the thermal properties of hexagonal transition metal dichalcogenide compounds with different average atomic masses but equivalent microstructures. Thermal conductivity values of sputtered thin films were compared to bulk crystals. The comparison revealed a >10 fold reduction in thin film thermal conductivity. Structural analysis of the films revealed a turbostratic structure with domain sizes on the order of 5-10 nm. Estimates of phonon scattering lengths at domain boundaries based on computationally derived group velocities were consistent with the observed film microstructure, and accounted for the reduction in thermal conductivity compared to values for bulk crystals.

36 MATERIALS SCIENCE↗

A New Method for Low Cost Production of Titanium Alloys for Reducing Energy Consumption of Mechanical Systems

This project investigated an innovative manufacturing process intended to minimize the cost of production of titanium materials and components, and increase the adoption of Ti components for energy consuming applications, such as automobiles. A key innovation of the proposed manufacturing approach is a novel Ti powder sintering technology for making titanium materials with ultrafine grain microstructure in the as-sintered state with minimum, or an absence, of post-sintering processes. The new sintering technology is termed Hydrogen Sintering and Phase Transformations (HSPT), and constitutes a promising manufacturing technology that can be used to produce titanium (Ti) materials and components in a near-net-shape form, thus also minimizing machining costs. Our objective was to meet, or possibly surpass, the mechanical property levels for ASTM B348 Grade 5 for wrought Ti-6Al-4V. Although specific applications call for varying mechanical property requirements, ASTM B348 was created for the demanding applications of the aerospace industry, and is the established standard for Ti-6Al-4V. While the primary goal was to meet, or exceed this standard, the team also had the goal of demonstrating this could be done at a significantly lower cost of production. Interim goals of the project were to fully develop this novel sintering process, and provide sufficient baseline testing to make the method practical and attractive to industry. By optimizing the process parameters for the sintering of titanium hydride (TiH 2 ) powders in a hydrogen atmosphere and controlling the phase transformations during and after sintering, the HSPT process was expected to reduce the energy consumption, and thus cost, of making Ti alloys and fabricating Ti components. The process was designed such that no high temperature melting is required for producing Ti alloys; little or no post-sintering processing is needed for producing desired microstructures (and therefore enhanced mechanical properties), and finally, minimum machining is needed to fabricate finished Ti components. An energy analysis within this report provides more detail, but calculated values indicate that the HSPT process is less than half as energy intensive as conventional wrought processing, while producing mechanical properties that are comparable. In addition to the energy savings anticipated from the industrial production of Ti components, a second prong of energy savings resides in the use phase of components produced, primarily from use in the transportation sector. Titanium has a number of material qualities appropriate for the auto industry, particularly low mass and corrosion resistance. By reducing the weight of automobiles and other vehicles, energy costs and CO 2 production will be reduced over the lifetime of the vehicles, and components in corrosive environments on vehicles, such as exhaust systems and other under carriage parts, may not have to be replaced during a vehicle’s lifetime. Our analysis indicates that by replacing only 5.6 kg of steel parts in an auto with Ti components across the entire US fleet would save approximately 486 million gallons of gasoline per year. This correlates to a reduction of 3.6 million metric tons of CO 2 per year. The potential for replacing many more of the steel parts in automobiles with lighter weight titanium components is clear. The project was very successful overall, meeting all milestones and surpassing project goals in terms of mechanical properties and microstructures produced. In addition to tensile properties, fatigue properties were emphasized in the project work. Powder metallurgy processes often have porosity to some degree in their final microstructure, and porosity is a well-known cause of crack initiation and low fatigue performance. Although many automobile applications do not undergo fatigue stress regimes, many others do encounter cyclic stress, and design criteria in the latter case require good fatigue properties. Production and testing of HSPT parts showed excellent tensile properties and fracture toughness, and fatigue properties that exceeded all previously reported powder metallurgy Ti methods, overlapping with wrought processed values. Fatigue limits exceeded 500 MPa and tensile strength exceeded 1,000 MPa while maintaining good ductility. Microstructures produced during the project period easily surpassed pre-project expectations. In addition to producing very fine grains in the as-sintered state (without post sintered thermo-mechanical work), porosity was reduced and industrially relevant microstructures previously undemonstrated in any other powder metallurgy titanium method were produced using HSPT materials. These microstructures, both bi-modal and globularized, were produced with simple post-sinter heat treatments, but without the need for energy intensive mechanical work. The employed heat treatments expanded the available mechanical property range (tensile strength vs. ductility) of the HSPT system in Ti-6Al-4V. The project has resulted in the publication, thus far, of five refereed journal articles and five conference proceedings papers, as well as a patent application, two dissertations and a master’s thesis. Two additional journal articles are currently under review, and at least three others are currently in preparation, with several additional students anticipated to graduate within the coming year. Presentations and papers were a particular focus of the second half of the project, once significant experimentation had been performed and analyzed. As part of our efforts to disseminate information of our results, the Ti research teams within Prof. Fang’s and Prof. Chandran’s research groups had a strong presence at the 13th World Conference on Ti, August 16-20, 2015, in San Diego. Several research groups in the US and in Europe are now performing experiments using the HSPT process. Accompanying efforts to bring HSPT to the Ti community at large, and industry in particular, work has continued with our partners and with other interested industrial Ti users and producers, including Boeing and GKN (a major powder metallurgy parts manufacturer). Commercialization has been a central focus of the final phase of the project, and Reading Alloys signed a provisional licensing agreement in summer of 2015. They are currently seeking an appropriate customer with which to pursue initial parts manufacturing efforts. Other licensing options and partners are continuing to be pursued. The promise of lightweight, strong and corrosion resistant Ti alloys with long fatigue lifetimes for automobile or transportation applications has been the vision of the metal industry since titanium came to the attention of scientists and engineers. The sole limitation of realizing these goals has been cost, which is primarily a function of energy used in production. The HSPT process was shown through this work to be capable of realizing this goal, and facilitating the practical use of titanium in US automotive and other industries.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

Fabrication of PbS nanoparticle coated amorphous carbon nanotubes: Structural, thermal and field emission properties

Graphical abstract: Simple chemical synthesis of PbS nanoparticle coated amorphous carbon nanotubes have shown better thermal stability and enhanced electron field emission properties. Highlights: {yields} PbS nanocrystals coated amorphous carbon nanotubes have been synthesized through a simple chemical route at low temperature. {yields} The composite is thermally more stable than amorphous CNTs. {yields} Composite have shown excellent cold cathode field emission property. -- Abstract: A simple chemical route for the synthesis of PbS nanoparticle coated amorphous carbon nanotubes (aCNTs) was described. The nanocomposite was prepared from an aqueous suspension of acid functionalized aCNTs, lead acetate (PbAc), and thiourea (TU) at room temperature. The phase formation and composition of the samples were characterized by X-ray diffraction and energy dispersive analysis of X-ray studies. The Fourier transformed infrared spectra analysis revealed the attachment of PbS nanoparticles on the acid functionalized aCNT surfaces. Morphology of the samples was analyzed with a field emission scanning electron microscope. UV-Vis study also confirmed the attachment of PbS nanoparticles on the walls of aCNTs. Thermal gravimetric analysis showed that the PbS coated aCNTs are more thermally stable than functionalized aCNTs. The PbS coated aCNTs showed enhanced field emission properties with a turn-on field 3.34 V {mu}m{sup -1} and the result is comparable to that of pure crystalline CNTs.

36 MATERIALS SCIENCE↗

Linking sintering stresses to nano modification in the microstructure of BaLa4Ti4O15 by transmission electron microscopy

Highlights: • by systematic HRTEM studies we link the microstructural changes in BLT ceramics to the external pressure applied during sintering; • we developed a mechanistic understanding of the role of stress in sintering; • external stresses during sintering affect the microstructural development at the nanoscale level, being responsible for the creation of higher defective bulk and grain boundary regions; • observation of high density of stacking faults (which generally arrises due to the Ti vacancy layers) indicates that the applied stress is modifying the stacking of AO{sub 3} layers of BLT which in turn creates Ti vacancy layer and stacking faults; • stress assisted sintering has, therefore, the potential to be used as a tool to design microstructures and achieve tailored properties, as suggested from our previous results in BLT and BNT. - Abstract: High quality factor and a temperature stable resonant frequency make BaLa{sub 4}Ti{sub 4}O{sub 15} (BLT) ceramics attractive materials for microwave applications. Aiming to exploit the effects of external stresses on the development of textured and anisotropic microstructures to optimise MW properties, the influence of applied external pressure during sintering of BLT ceramics is analysed. HRTEM and geometric phase analysis (GPA) showed that stresses applied during sintering, trigger the nucleation and growth of faults hypothesised to be due to the errors in the AO{sub 3} layer (basal plane) stacking sequence of the hexagonal perovskite structure. The results reveal a strong correlation between the high concentration of structural defects and the development of anisotropic microstructures, which tune the properties of BLT. Stresses applied during sintering are therefore a promising tool to design material properties.

36 MATERIALS SCIENCE↗