Low-thermal-budget solution processing of thin films of zinc ferrite and other complex oxides

Further miniaturization of magnetic and electronic devices demands thin films of advanced nanomaterials with unique properties. Spinel ferrites have been studied extensively owing to their interesting magnetic and electrical properties coupled with stability against oxidation. Being an important ferrospinel, zinc ferrite has wide applications in the biological (MRI) and electronics (RF-CMOS) arenas. The performance of an oxide like ZnFe2O4 depends on stoichiometry (defect structure), and technological applications require thin films of high density, low porosity and controlled microstructure, which depend on the preparation process. While there are many methods for the synthesis of polycrystalline ZnFe2O4 powder, few methods exist for the deposition of its thin films, where prolonged processing at elevated temperature is not required. We report a novel, microwave-assisted, low temperature (<100°C) deposition process that is conducted in the liquid medium, developed for obtaining high quality, polycrystalline ZnFe2O4 thin films on technologically important substrates like Si(100). An environment-friendly solvent (ethanol) and non-hazardous oxide precursors (β-diketonates of Zn and Fe in 1:2 molar ratio), forming a solution together, is subjected to irradiation in a domestic microwave oven (2.45 GHz) for a few minutes, leading to reactions which result in the deposition of ZnFe2O4 films on Si (100) substrates suspended in the solution. Selected surfactants added to the reactant solution in optimum concentration can be used to control film microstructure. The nominal temperature of the irradiated solution, i.e., film deposition temperature, seldom exceeds 100°C, thus sharply lowering the thermal budget. Surface roughness and uniformity of large area depositions (50x50 mm2) are controlled by tweaking the concentration of the mother solution. Thickness of the films thus grown on Si (100) within 5 min of microwave irradiation can be as high as several microns. The present process, not requiring a vacuum system, carries a very low thermal budget and, together with a proper choice of solvents, is compatible with CMOS integration. This novel solution-based process for depositing highly resistive, adherent, smooth ferrimagnetic films on Si (100) is promising to RF engineers for the fabrication of passive circuit components. It is readily extended to a wide variety of functional oxide films.

New metal-organic precursors for MOCVD applications: Synthesis, characterization, crystal structure and thermal properties of mixed-ligand Mg(II) complexes

In an effort to develop new MOCVD precursors, mixed-ligand metal-organic complexes, bis (acetylacetonato-k(2)O,O') (2,2'-bipyridine-k(2)N,N') magnesium(II), and his (acetylacetonato-k(2)O,O') (1,10-phenanthroline-k(2)N,N') magnesium(II) were synthesized. Spectroscopic characterization and crystal structures confirmed them to be monomeric and stable complexes. Crystal structure analysis suggests in each of the magnesium(II) complexes, the metal center has a distorted octahedral coordination geometry. Thermo-gravimetric analysis (TGA/DTA) suggests that these complexes are volatile and thermally stable. The thermal characteristics of newly designed complexes make them attractive precursors for MOCVD applications. (c) 2012 Elsevier B.V. All rights reserved.

Self catalytic growth of SnO2 branched nanowires by thermal evaporation

For the first time, Tin oxide (SnO2) multiple branched nanowires (NWs) have been synthesized by thermal evaporation of tin (Sn) in presence of oxygen without use of metal catalysts at low substrate temperature of 500 degrees C. Synthesized product consists of multiple branched nanowires and were single crystalline in nature. Each of the nanowire capped with catalyst particle at their ends. Energy dispersive X-ray analysis on the nanowires and capped nanoparticle confirms that Sn act as catalyst for SnO2 nanowires growth. A self catalytic vapor-liquid-solid (VLS) growth mechanism was proposed to describe the SnO2 nanowires growth. (C) 2012 Elsevier B.V. All rights reserved.

Thermal Rearrangement of Azido Ketones into Oxazoles via Azirines: One-Pot, Metal-Free Heteroannulation to Functionalized 1,3-Oxazoles

alpha-Azidoacetophenones were converted into 2-aryl-1,3-oxazole-4-carbaldehydes through rearrangement of the carbon framework upon exposure to DMF/POCl3. The unprecedented rearrangement occurs via alkenyl azides and 2H-azirines. A mechanism for this unusual reaction was proposed and evidenced.

Proportional resonant controller based circulating power setup for thermal testing of multilevel inverter

A regenerative or circulating-power method is presented in this paper for heat run test on the legs of a three-level neutral point clamped (NPC) inverter. This test ensures that only losses are drawn from the dc supply, while rated power is circulated between the two legs, thus minimising wastage of energy. A proportional-resonant (PR) controller based current control scheme is proposed here for the circulating power test setup in NPC inverter. Simulation and experimental results are presented to validate the controller design at various operating conditions. Results of thermal test on the inverter legs are presented at two different operating conditions.

Experiments on thermal response of low aspect ratio packed beds at high Reynolds numbers with varying inflow temperature

An experimental study for transient temperature response of low aspect ratio packed beds at high Reynolds numbers for a free stream with varying inlet temperature is presented. The packed bed is used as a compact heat exchanger along with a solid propellant gas-generator, to generate room temperature gases for use in applications such as control actuation and air bottle pressurization. Packed beds of lengths similar to 200 mm and 300 mm were characterized for packing diameter based Reynolds numbers, Re-d ranging from 0.6 x 10(4) to 8.5 x 10(4). The solid packing used in the bed consisted of circle divide 9.5 mm and circle divide 5 mm steel spheres with suitable arrangements to eliminate flow entrance and exit effects. The ratios of packed bed diameter to packing diameter for 9.5 mm and 5 mm sphere packing were similar to 9.5 and 18 respectively, with the average packed bed porosities around 0.4. Gas temperatures were measured at the entry, exit and at three axial locations along centre-line in the packed beds. The solid packing temperature was measured at three axial locations in the packed bed. An average Nusselt number correlation of the form Nu(d) = 3.91Re(d)(05) for Re-d range of 10(4) is proposed. For engineering applications of packed beds such as pebble bed heaters, thermal storage systems, and compact heat exchangers a simple procedure is suggested for calculating unsteady gas temperature at packed bed exit for packing Biot number Bi-d < 0.1. (C) 2012 Elsevier Inc. All rights reserved.

Method for Seismic Microzonation with Geotechnical Aspects

This study presents an overview of seismic microzonation and existing methodologies with a newly proposed methodology covering all aspects. Earlier seismic microzonation methods focused on parameters that affect the structure or foundation related problems. But seismic microzonation has generally been recognized as an important component of urban planning and disaster management. So seismic microzonation should evaluate all possible hazards due to earthquake and represent the same by spatial distribution. This paper presents a new methodology for seismic microzonation which has been generated based on location of study area and possible associated hazards. This new method consists of seven important steps with defined output for each step and these steps are linked with each other. Addressing one step and respective result may not be seismic microzonation, which is practiced widely. This paper also presents importance of geotechnical aspects in seismic microzonation and how geotechnical aspects affect the final map. For the case study, seismic hazard values at rock level are estimated considering the seismotectonic parameters of the region using deterministic and probabilistic seismic hazard analysis. Surface level hazard values are estimated considering site specific study and local site effects based on site classification/characterization. The liquefaction hazard is estimated using standard penetration test data. These hazard parameters are integrated in Geographical Information System (GIS) using Analytic Hierarchy Process (AHP) and used to estimate hazard index. Hazard index is arrived by following a multi-criteria evaluation technique - AHP, in which each theme and features have been assigned weights and then ranked respectively according to a consensus opinion about their relative significance to the seismic hazard. The hazard values are integrated through spatial union to obtain the deterministic microzonation map and probabilistic microzonation map for a specific return period. Seismological parameters are widely used for microzonation rather than geotechnical parameters. But studies show that the hazard index values are based on site specific geotechnical parameters.

Thermal vibration analysis of monolayer graphene embedded in elastic medium based on nonlocal continuum mechanics

This paper presents the thermal vibration analysis of single-layer graphene sheet embedded in polymer elastic medium, using the plate theory and nonlocal continuum mechanics for small scale effects. The graphene is modeled based on continuum plate theory and axial stress caused by the thermal effects is also considered. Nonlocal governing equation of motion for this graphene sheet system is derived from the principle of virtual displacements. The closed form solution for thermal-vibration frequencies of a simply supported rectangular nanoplate has been obtained by using the Navier's method of solution. Numerical results obtained by the present theory are compared with available solutions in the literature and the molecular dynamics results. The influences of the small scale coefficient, the room or low temperature, the high temperature, the half wave number and the aspect ratio of nanoplate on the natural frequencies are considered and discussed in detail. The thermal vibration analysis of single- and double-layer graphene sheets are considered for the analysis. The mode shapes of the respective graphene system are also captured in this work. The present analysis results can be used for the design of the next generation of nanodevices that make use of the thermal vibration properties of the graphene.

Study of thermal relaxation of Poly (HDDA-co-MMA) by temperature modulated DSC and dielectric spectroscopy

The thermal transitions in the copolymer of 1,6-hexanediol diacrylate (HDDA) and methyl methacrylate (MMA) was investigated to understand its use in microstereolithography. The glass transition temperature and the effect of interaction on this transition process was investigated by means of temperature modulated differential scanning calorimetry (TMDSC). The heat capacities were determined and PHDDA rich phases showed lower heat capacity than PMMA rich phases. The frequency dependence of glass transitions were studied by varying the modulation period of TMDSC and confirmed by dielectric relaxation spectroscopy. Vogel Fulcher Tammann Hesse (VFTH) parameters of homo and copolymers have also been reported.

Growth and characterization of micro and nanostructures of lead telluride (PbTe) by thermal evaporation method

Lead telluride micro and nanostructures have been grown on silicon and glass substrates by a simple thermal evaporation of PbTe in high vacuum of 3 x 10(-5) mbar. Growth was carried out for two different distances between the evaporation source and the substrates. Synthesized products consist of nanorods and micro towers for 2.4 cm and 3.4 cm of distance between the evaporation source and the substrates respectively. X-ray diffraction and transmission electron microscopy studies confirmed crystalline nature of the nanorods and micro towers. Nanorods were grown by vapor solid mechanism. Each micro tower consists of nano platelets and is capped with spherical catalyst particle at their end, suggesting that the growth proceeds via vapor-liquid-solid (VLS) mechanism. EDS spectrum recorded on the tip of the micro tower has shown the presence of Pb and Te confirming the self catalytic VLS growth of the micro towers. These results open up novel synthesis methods for PbTe nano and microstructures for various applications.

Synthesis, microstructure and thermal expansion studies on Ca0 center dot 5+x/2Sr0 center dot 5+x/2Zr4P6-2x Si-2x O-24 system prepared by co-precipitation method

We report on the synthesis, microstructure and thermal expansion studies on Ca0 center dot 5 + x/2Sr0 center dot 5 + x/2Zr4P6 -aEuro parts per thousand 2x Si-2x O-24 (x = 0 center dot 00 to 1 center dot 00) system which belongs to NZP family of low thermal expansion ceramics. The ceramics synthesized by co-precipitation method at lower calcination and the sintering temperatures were in pure NZP phase up to x = 0 center dot 37. For x a parts per thousand yen 0 center dot 5, in addition to NZP phase, ZrSiO4 and Ca2P2O7 form as secondary phases after sintering. The bulk thermal expansion behaviour of the members of this system was studied from 30 to 850 A degrees C. The thermal expansion coefficient increases from a negative value to a positive value with the silicon substitution in place of phosphorous and a near zero thermal expansion was observed at x = 0 center dot 75. The amount of hysteresis between heating and cooling curves increases progressively from x = 0 center dot 00 to 0 center dot 37 and then decreases for x > 0 center dot 37. The results were analysed on the basis of formation of the silicon based glassy phase and increase in thermal expansion anisotropy with silicon substitution.

Nanocomposites of crosslinked starch phthalate and silane modified nanoclay: Study of mechanical, thermal, morphological, and biodegradable characteristics

Biodegradable composites comprising of modified starch and modified nanoclay have been prepared. Starch has been modified by esterification and subsequently crosslinked. The thermal, mechanical, and biodegradation characteristics of the composites have been investigated. The compressive properties of the composites with the addition of nanoclay were twice that of crosslinked starch phthalate without addition of nanoclay. Predictive theories were used to analyze the obtained experimental results. SEM studies on fracture morphology indicated quasi-brittle fracture. Flexural properties showed considerable improvement due to nanoclay addition. The water uptake increased up to 6% nanoclay, beyond which the uptake decreased. Biodegradation studies showed an initial time lag prior to the onset of degradation.

Influence of steric effect on the structural aspects of N,N `,N `'-triarylguanidine derived six-membered C,N] palladacycles

Guanidine derived six-membered C,N] palladacycles of the types (C,N)Pd(mu-OC(O)R)](2) (1a-d), (C,N)Pd(mu-Br)](2) (2a,b), cis-(C,N)PdBr(L)] (3a-d, 4, and 5), and ring contracted guanidine derived five-membered C,N] palladacycle, (C,N)PdBr(C NXy)] (6) were prepared in high yield following the established methods with a view aimed at understanding the influence of the substituents on the aryl rings of the guanidine upon the solid state structure and solution behaviour of palladacycles. Palladacycles were characterised by microanalytical, IR, NMR and mass spectral data. The molecular structures of 1a, 1c, 2a, 2b, 3a, 3c, 3d, and 4-6 were determined by single crystal X-ray diffraction data. Palladacycles 1a and 1c were shown to exist as a dimer in transoid in-in conformation in the solid state but as a mixture of a dimer in major proportion and a monomer (kappa(2)-O,O'-OAc) in solution as deduced from H-1 NMR data. Palladacycles 2a and 2b were shown to exist as a dimer in transoid conformation in the solid state but the former was shown to exist as a mixture of a dimer and presumably a trimer in solution as revealed by a variable temperature H-1 NMR data in conjunction with ESI-MS data. The cis configuration around the palladium atom in 3a, 3c, and 3d was ascribed to steric influence of the aryl moiety of =NAr unit and that in 4-6 was ascribed to antisymbiosis. The solution behaviour of 3d was studied by a variable concentration (VC) H-1 NMR data.

Hardening and corrosion behaviour of copper added SUS 304H austenitic steels subjected to thermal cycling

This research was aimed at determining optimum Cu content for the alloy design of SUS 30411 austenitic steels having enhanced heat and corrosion resistance. Samples of the steel containing 1, 3, and 5 wt.% Cu were subjected to repeated heating and cooling to a temperature of 760 degrees C and to a maximum of 15 cycles. Hardness measurement and the corrosion behaviour in 1M NaCl solution were evaluated. The hardness increases with an increase in the number of heating cycles for the three compositions. The hardening response to the thermal cycles is however higher for the 1 wt.% Cu composition and decreases with an increase in the Cu wt.%. The SUS 30411 steel containing 3 wt.% Cu exhibited the least susceptibility to corrosion in the 1M NaCl solution irrespective of the number of heating cycles. The SUS 30411 steel containing 1 wt.% Cu was found to exhibit the highest susceptibility to corrosion for all heating cycles compared.

Effect of thermal and thermo-mechanical cycling on the microstructure of Ni-rich NiTi shape memory alloys

Microstructural changes of Ni-rich NiTi shape memory alloy during thermal and thermo-mechanical cycling have been investigated using Electron Back Scattered Diffraction. A strong dependence of the orientation of the prior austenite grain on the misorientation development has been observed during thermal cycling and thermo-mechanical cycling. This effect is more pronounced at the grain boundaries compared to grain interior. At a larger applied strain, the volume fraction of stabilized martensite phase increases with increase in the number of cycling. Deformation within the martensite leads to stabilization of martensitic phase even at temperatures slightly above the austenite finish temperature. Modulus variation with respect to temperature has been explained on the basis of martensitic transformation.