Influence of sintering conditions and doping on the dielectric relaxation originating from the surface layer effects in CaCu3Ti4O12 ceramics

Detailed investigations into the dielectric dispersion phenomenon in the giant dielectric constant material CaCu3Ti4O12 (CCTO) around room temperature revealed the existence of two successive dielectric relaxations. In the temperature domain, a new dielectric relaxation was clearly observed around 250K, in addition to the well-investigated dielectric relaxation close to 100K. The effect of sintering and doping (La3+) on the strength of these dielectric relaxations were studied in detail. The sintering temperature as well as its duration was found to have tremendous influence on the dielectric relaxation that was encountered around 250 K. This Maxwell-Wagner (M-W) type of relaxation was found to be originating from the surface layer containing the Cu-rich phase, which was ascribed to the difference in the oxygen content between the surface and the interior of the sample. Interestingly, this particular additional relaxation was not observed in La2/3Cu3Ti4O12, a low dielectric constant member of the CCTO family, in which the segregation of Cu-rich phase on the surface was absent. Indeed the correlation between the new relaxation and the presence of Cu-rich phase in CCTO ceramics was further corroborated by the absence of the same after removing the top and bottom layers. (C) 2007 Elsevier Ltd. All rights reserved.

Studies on the ignition behaviour of boron powder

The ignition behaviour of boron powder, prepared through electrowinning process, was studied by using thermogravimetry coupled with simultaneous differential thermal analysis (TG-SDTA). The dependence of the inception of the ignition reaction on the partial pressure of oxygen, particle size of the boron powder and heating rate was investigated. It was observed that all these factors affect the ignition temperature. Boron powder with a mean particle size of about 10 mu m was found to be susceptible to ignition in oxygen even at 783K. In general, the susceptibility to ignition was found to vary inversely with the degree of crystallinity. Presence of carbon was found to retard the oxidation of boron and raise the ignition temperature. These results are useful in safe handling and storage of finely divided boron powder and in the subsequent production of boron carbide from it. (C) 2009 Elsevier B.V. All rights reserved.

Synthesis, sintering and microstructural characterization of nanocrystalline Hydroxyapatite Composites

Nanocrystalline hydroxyapatite (HAp) exhibits better bioactivity and biocompatibility with enhanced mechanical properties compared to the microcrystalline counterpart. In the present work, nanocrystalline hydroxyapatite was synthesized by wet chemical method. Sintering was carried out with nanocrystalline alumina as additive, the content of alumina being varied from 10 to 30 wt% in the composite. For 20 and 30 wt % Al2O3, hydroxyapatite decomposed into tricalcium phosphate (TCP) above the sintering temperature of 1100 degrees C. The fracture toughness of nano HAp-nano Al2O3 composite is anisotropic in nature and reached a maximum value of 6.9 MPa m(1/2).

A coaxial capacitive voltage divider for oscilloscopic recording of nanosecond high voltage pulses

A coaxial capacitance voltage divider with a ratio of 110 and a rise time much less than 2.5 ns was developed for use with a transmission line pulse generator capable of producing 100 kV rectangular pulses of 2 mu s duration. The low voltage arm of the divider is a 3 cm long tube of titania (TiO2) turned out from a cylindrical compact. The compact was made by first pressing titania powder using a suitable binder and then sintering at controlled temperatures. The tube was slipped over the terminating end of the pulse-forming cable to form the divider with the cable capacitance.

Surface diffusion driven nanoshell formation by controlled sintering of mesoporous nanoparticle aggregates

We report a general method for the synthesis of hollow structures of a variety of functional inorganics by partial sintering of mesoporous nanocrystal aggregates. The formation of a thin shell initiates the transport of mass from the interior leading to growth of the shell. The principles are general and the hollow structures thus produced are attractive for many applications including catalysis, drug delivery and biosensing.

Effect of sintering on optical, structural and photoluminescence properties of ZnO thin films prepared by sol-gel process

Zinc oxide (ZnO) thin films have been deposited on glass substrates via sol-gel technique using zinc acetate dihydrate as precursor by spin coating of the sol at 2000 rpm. Effects of annealing temperature on optical, structural and photo luminescence properties of the deposited ZnO films have been investigated. The phase transition from amorphous to polycrystalline hexagonal wurtzite structure was observed at an annealing temperature of 400 degrees C. An average transmittance of 87% in the visible region has been obtained at room temperature. The optical transmittance has slightly increased with increase of annealing temperature. The band gap energy was estimated by Tauc's method and found to be 3.22 eV at room temperature. The optical band gap energy has decreased with increasing annealing temperature. The photoluminescence (PL) intensity increased with annealing temperature up to 200 degrees C and decreased at 300 degrees C. (c) 2010 Elsevier B.V. All rights reserved.

Functional nanoporous structures by partial sintering of nanorod assemblies

We present a general method for the synthesis of functional nanoporous structures by heat treating a loose compact of nanorods. Partial sintering of such a compact leads to spherodization of the nanorods and their fusion at the contact regions leading to an interconnected porous microstructure. The pore diameter can be controlled by changing the original nanorod diameter. We illustrate the generality of the method using TiO2, ZnO and hydroxyapatite as model systems; the method is applicable for any material that can be grown in the form of nanorods. The kinetics of the sintering process can be significantly enhanced in systems in which additional driving forces for mass transport arise from phase transitions proving an ultrafast pathway for producing biphasic porous structures. The possibility of producing hierarchical porous structures using fugitive sintering aids makes this process ideal for a variety of applications including catalysis, photoanodes for solar cells and scaffolds for biomedical applications.

C-H…O hydrogen bond mediated chain reversal in a peptide containing g-amino acid residue, determined directly from powder X-ray diffraction data

The finding that peptides containing -amino acid residues give rise to folding patterns hitherto unobserved in -amino acid peptides[1] has stimulated considerable interest in the conformational properties of peptides built from , and residues,[2] as the introduction of additional methylene (CH2) units into peptide chains provides further degrees of conformational freedom.

Towards Understanding Powder Behavior Via Simulation

The aim of this study was to investigate powder and tablet behavior at the level of mechanical interactions between single particles. Various aspects of powder packing, mixing, compression, and bond formation were examined with the aid of computer simulations. The packing and mixing simulations were based on spring forces interacting between particles. Packing and breakage simulations included systems in which permanent bonds were formed and broken between particles, based on their interaction strengths. During the process, a new simulation environment based on Newtonian mechanics and elementary interactions between the particles was created, and a new method for evaluating mixing was developed. Powder behavior is a complicated process, and many of its aspects are still unclear. Powders as a whole exhibit some aspects of solids and others of liquids. Therefore, their physics is far from clear. However, using relatively simple models based on particle-particle interaction, many powder properties could be replicated during this work. Simulated packing densities were similar to values reported in the literature. The method developed for describing powder mixing correlated well with previous methods. The new method can be applied to determine mixing in completely homogeneous materials, without dividing them into different components. As such, it can describe the efficiency of the mixing method, regardless of the powder's initial setup. The mixing efficiency at different vibrations was examined, and we found that certain combinations of amplitude, direction, and frequencies resulted in better mixing while using less energy. Simulations using exponential force potentials between particles were able to explain the elementary compression behavior of tablets, and create force distributions that were similar to the pressure distributions reported in the literature. Tablet-breaking simulations resulted in breaking strengths that were similar to measured tablet breaking strengths. In general, many aspects of powder behavior can be explained with mechanical interactions at the particle level, and single particle properties can be reliably linked to powder behavior with accurate simulations.

Interfacial Phenomena in Pharmaceutical Low Moisture Content Powder Processing

Powders are essential materials in the pharmaceutical industry, being involved in majority of all drug manufacturing. Powder flow and particle size are central particle properties addressed by means of particle engineering. The aim of the thesis was to gain knowledge on powder processing with restricted liquid addition, with a primary focus on particle coating and early granule growth. Furthermore, characterisation of this kind of processes was performed. A thin coating layer of hydroxypropyl methylcellulose was applied on individual particles of ibuprofen in a fluidised bed top-spray process. The polymeric coating improved the flow properties of the powder. The improvement was strongly related to relative humidity, which can be seen as an indicator of a change in surface hydrophilicity caused by the coating. The ibuprofen used in the present study had a d50 of 40 μm and thus belongs to the Geldart group C powders, which can be considered as challenging materials in top-spray coating processes. Ibuprofen was similarly coated using a novel ultrasound-assisted coating method. The results were in line with those obtained from powders coated in the fluidised bed process mentioned above. It was found that the ultrasound-assisted method was capable of coating single particles with a simple and robust setup. Granule growth in a fluidised bed process was inhibited by feeding the liquid in pulses. The results showed that the length of the pulsing cycles is of importance, and can be used to adjust granule growth. Moreover, pulsed liquid feed was found to be of greater significance to granule growth in high inlet air relative humidity. Liquid feed pulsing can thus be used as a tool in particle size targeting in fluidised bed processes and in compensating for changes in relative humidity of the inlet air. The nozzle function of a two-fluid external mixing pneumatic nozzle, typical for small scale pharmaceutical fluidised bed processes, was studied in situ in an ongoing fluidised bed process with particle tracking velocimetry. It was found that the liquid droplets undergo coalescence as they proceed away from the nozzle head. The coalescence was expected to increase droplet speed, which was confirmed in the study. The spray turbulence was studied, and the results showed turbulence caused by the event of atomisation and by the oppositely directed fluidising air. It was concluded that particle tracking velocimetry is a suitable tool for in situ spray characterisation. The light transmission through dense particulate systems was found to carry information on particle size and packing density as expected based on the theory of light scattering by solids. It was possible to differentiate binary blends consisting of components with differences in optical properties. Light transmission showed potential as a rapid, simple and inexpensive tool in characterisation of particulate systems giving information on changes in particle systems, which could be utilised in basic process diagnostics.