Fabrication of submicron alumina ceramics by pulse electric current sintering using M2+ (M = Mg,Ca, Ni)-doped alumina nanopowders

Dense submicron-grained alumina ceramics were fabricated by pulse electric current sintering (PECS) using M²⁺(M: Mg, Ca, Ni)-doped alumina nanopowders at 1250 °C under a uniaxial pressure of 80 MPa. The M²⁺-doped alumina nanopowders (0–0.10 mass%) were prepared through a new sol–gel route using high-purity polyhydroxoaluminum (PHA) and MCl₂ solutions as starting materials. The composite gels obtained were calcined at 900 °C and ground by planetary ball milling. The powders were re-calcined at 900 °C to increase the content of α-alumina particles, which act as seeding for low-temperature densification. Densification and microstructural development depend on the M²⁺ dopant species. Dense alumina ceramics (relative density ≥99.0%) thus obtained had a uniform microstructure composed of fine grains, where the average grain size developed for non-doped, Ni-doped, Mg-doped and Ca-doped samples was 0.67, 0.67, 0.47 and 0.30 μm, respectively, showing that Ca-doping is the most promising method for tailoring of nanocrystalline alumina ceramics.     

Preparation of novel porous solids from alumina-pillared fluorine micas by acid-treatment

New porous solids from alumina-pillared fluorine micas (APMs), which were obtained from synthetic Na-tetrasilicic fluorine mica [NaMg_2.5Si₄O₁₀F₂], were prepared by sulfuric acid-treatment under mild conditions at 25 °C. The products were investigated by XRD, ICP, SEM, TEM and N₂ adsorption–desorption isotherm at 77 K. XRD measurements indicated that the interlayer pillared structure having a large basal spacing collapsed during the early stages of the acid-treatment. ICP analyses indicated that Al³⁺ and Mg²⁺ ions were leached out from the pillared micas during the acid-treatment. The pore properties of the leached products were found to differ from those of the mother pillared micas: the acid leaching of the pillared micas leads to the formation of mesopores around 3.2 nm in diameter. The correlation between the change in pore properties and cation elution behavior suggests that the mesopore formation results from the leaching of Mg²⁺ ions from the octahedral sheet of the pillared micas. The leached products thus obtained retained the flaky morphology of the mother pillared micas. These results show that the mild acid-treatment using APMs provides a novel route for obtaining unique mesopore solids having the large particle sizes of the mother micas.     

Nanocrystallization of Fe73.5Si13.5B9Nb3Cu1 soft-magnetic alloy from amorphous precursor in a magnetic field

The effect of a magnetic field on the nature of nanocrystallization from a melt-spun Fe_73.5Si_13.5B₉Nb₃Cu₁ amorphous precursor has been studied with the aim of controlling microstructures and magnetic properties. Annealing for magnetic crystallization was carried out at temperatures between the Curie temperature of the amorphous phase (586 K) and that of the crystalline phase (920 K). It was found that the {110} texture component in crystallized α-Fe(Si) phase increased in importance with increasing magnetic-field strength. An X-ray diffraction analysis based on the Shultz method revealed that the magnetic field caused preferential formation of {110}-oriented nuclei. In addition, the applied field enhanced crystallization kinetics, particularly the nucleation rate. No significant difference in grain growth behavior was observed as a result of applying a magnetic field. We therefore conclude that the development of the {110} texture by magnetic crystallization is predominantly attributable to preferential nucleation, rather than preferential growth, of {110}-oriented nuclei. The saturation magnetization of nanocrystallized specimens, evaluated using a vibrating sample magnetometer (VSM), was increased by the application of a magnetic field up to 4T during nanocrystallization.     

A Nifedipine Coground Mixture with Sodium Deoxycholate. II. Dissolution Characteristics and Stability

Nifedipine is a poorly water soluble drug that demonstrates low bioavailability. In a previous study, a coground mixture of nifedipine with sodium deoxycholate (DCNa), a bile salt, immediately produced colloidal particles when dispersed in water. In this study, the effect of the weight fraction of DCNa, grinding time, dissolution media, and storage conditions on colloidal particle formation in solution was investigated. The coground mixture was prepared with a vibration rod mill, and its solid state was characterized using powder X-ray diffraction. A laser diffraction particle size analyzer was used to determine the particle size distribution curve in water. The size of particles formed in solution decreased with an increase in the weight fraction of DCNa and grinding time. A nifedipine-DCNa (1 : 2 w/w) mixture coground for 30 min was used in the experiments. Colloidal particle formation from the coground mixture was also observed in dissolution media of water and a pH 6.8 buffer solution at 37°C. Most precipitates passed through a filter with a pore size of 0.8 μm, but the particle size distribution in water was different from that in the pH 6.8 buffer solution. DCNa exhibited not only micellar solubilization for drug crystals, but also a retarding effect on drug crystal growth in a supersaturated solution. The latter effect could serve to form colloidal particles in solution. When stored under 75% relative humidity at 40°C for 1 month, the amorphous coground mixture crystallized, and the particle size in water markedly increased. Therefore, the weight fraction of DCNa, grinding time, dissolution media, and humidity during storage influence the dissolution characteristics of nifedipine from a coground mixture.     

Crystal growth of MgAlB14-type compounds using metal salts and some properties

LEAlB₁₄ (orthorhombic, Imam) (LE = Li, Mg) crystals were grown using metal salts (Li₂CO₃, LiF, LiI, MgO, MgF₂, MgI₂) and crystalline boron from a high-temperature aluminium metal flux. The growth conditions for growing LEAlB₁₄ were established using the starting mixtures of B/LE = 2.0, and Al metal was added to each mixture at a mass ratio of 1:15–20. LEAlB₁₄ crystals from the Al-self flux using metal salts could be obtained from all the different salts. The maximum dimensions of LiAlB₁₄ and MgAlB₁₄ crystals were approximately 18 and 12 mm for the crystals obtained from LiF and MgF₂. The unit-cell parameters of as-grown LEAlB₁₄ are as follows: for LiAlB₁₄, obtained from LiF, a = 0.5846 (2) nm, b = 0.8144 (2) nm, c = 1.0355 (3) nm, V = 0.4930 (2) nm³: for MgAlB₁₄, obtained from MgF₂, a = 0.5845 (2) nm, b = 0.8114 (2) nm, c = 1.0330 (3) nm, V = 0.4899 (3) nm³. Microhardness, oxidation resistance and magnetic susceptibility of these materials are described in detail.     

Speed-up of computing time for numerical analysis of particle charging process by using discrete element method

The objective of this paper is to improve the computing time for numerical analysis of particle charging process by using discrete element method. The rule for ignoring the calculations of contact forces and updating trajectories of unmoved particles were discussed. When the relative displacement of a particle within certain calculation steps became less than 0.1% of particle radius, this particle was determined to be unmoved and the calculations of this particle were ignored. The computing time was improved significantly when this new method was used, and its calculation speed was more than two times faster than that of original. It was found that this speed-up method is more useful for the cases that the particle becomes unmoved in short time or the height of charged bed is large. The simulation of charging process in an industrial-scale surge hopper was studied by using new method, the calculation speed became 2.88 times faster than that of original, and the quite similar particle size segregation between original and new methods was given. This new method for speed-up of the charging process in DEM is very useful, and the charging processes of the industrial scale storages can be simulated by using this method.     

In situ time-resolved X-ray diffraction of tobermorite formation in autoclaved aerated concrete: Influence of silica source reactivity and Al addition

The hydrothermal formation of tobermorite during the processing of autoclaved aerated concrete was investigated by in situ X-ray diffraction (XRD) analysis. High-energy X-rays from a synchrotron radiation source in combination with a newly developed autoclave cell and a photon-counting pixel array detector were used.To investigate the effects of the silica source, reactive quartz from chert and less-reactive quartz from quartz sand were used as starting materials. The effect of Al addition on tobermorite formation was also studied. In all cases, C-S-H, hydroxylellestadite and katoite were clearly observed as intermediates.Acceleration of tobermorite formation by Al addition was clearly observed. However, Al addition did not affect the dissolution rate of quartz. Two pathways, via C-S-H and katoite, were also observed in the Al-containing system. These results suggest that the structure of initially formed C-S-H is important for the subsequent tobermorite formation reactions.     

Multi-component granulation in a fast fluidized bed

The granulation of multi-component particles was conducted in a fast fluidized bed with an atomizing binder solution. The effects of gas velocity and binder droplet diameter on granulation rate, granule size distribution and granule composition were studied. The granulation rate and granule yield were determined by the balance between the agglomeration rate of feed particles and the disintegration rate of granules because there was no secondary granulation. With the increase in gas velocity and the reduction in binder droplet size, the agglomeration rate of feed particles decreased but the disintegration rate of granules increased, resulting in a reduced granule yield. Despite the larger fraction of small particles in the granules, the homogenous granulation of multi-component particles was achieved.     

Study on the hydrothermal drying technology of sewage sludge

Drying of sewage sludge is an effective way for treatment and utilization of sewage sludge,where reduction of energy consumption is one of the major technical challenges.So we experimentally investigated the possibility of the hydrothermal treatment.We have found that treatment of sewage sludge by saturated steam with the temperature of 190°C and pressure of 20 bar can dramatically improve the dehydration performance of the slurry like product.And the water content can be reduced down to about 55% by a mech...     

Methanol decomposition to synthesis gas over supported Pd catalysts prepared from synthetic anionic clays

Supported Pd or Rh catalysts were prepared by the solid-phase crystallization method starting from hydrotalcite anionic clay minerals based on [Mg₆Al₂(OH)₁₆CO ₂ ²⁻ ]·4H₂O as the precursors. The precursors were prepared by a coprecipitation method from the raw materials containing Pd²⁺ and various trivalent metal ions which can replace each site of Mg²⁺ and Al³⁺ in the hydrotalcite. Rh³⁺ was also used for preparing the catalyst as comparison. The precursors were then thermally decomposed and reduced to form supported Pd or Rh catalysts and used for the methanol decomposition to synthesis gas. Among the precursors tested, use of Mg–Cr hydrotalcite containing Pd²⁺ resulted in the formation of efficient Pd supported catalysts for the production of synthesis gas by selective decomposition of methanol at low temperature. Although Pd²⁺ cannot well replace the Mg²⁺ site in the hydrotalcite, the Pd supported catalyst (Pd/Mg–Cr) prepared by the solid-phase crystallization method formed highly dispersed Pd metal particles and showed much higher activity than that prepared by the conventional impregnation method. When the precursor was prepared under mild conditions, more fine particles of Pd metal were formed over the catalyst, resulting in high activity. It is likely that the high activity may be due to the highly dispersed and stable Pd metal particles assisted by the role of Cr as the co-catalyst. This revised version was published online in November 2006 with corrections to the Cover Date.