Effect of morphology and particle size on the ionic conductivities of composite solid electrolytes

A model incorporating the surface conductivity and morphology of the composite solid electrolytes is envisaged to explain their conduction behaviour. The conductivity data on LinX−50 m/o Al2O3 (X = F−, Cl−, Br−, CO32−, SO42−, PO43−) composites prepared by thermal decomposition of LinX·2nAl(OH)3·mH2O salts and Li2SO4−A (A=Al2O3, CeO2, Y2O3, Yb2O3, Zr2O3, ZrO2 and BaTiO3) composites prepared by mechanical mixing of the components are examined in the light of this model. It is surmised that the particle size of both the dispersoids and the hosts not only influence the ionic conductivity of the host matrix but also affect its bulk properties.

Temperature programmed desorption studies on hydrodesulfurization catalysts

The temperature programmed-desorption (TPD) of butane, butene, butadiene and thiophene over a series of Co-MO/gamma-Al2O3 catalysts with varying Co to Mo ratio has been investigated. The TPD of butane, butene and butadiene over catalysts containing no Co showed a single desorption profile while incorporation of Co created an additional site without significantly affecting desorption from the original site. The TPD of thiophene over a series of catalysts with varying Co content showed identical desorption temperature as well as heat of desorption. It was concluded that thiophene was adsorbed on the ''Mo-S'' component of the catalyst and was unaffected by the presence of Co.

The role of additives in a complex lithium silicate glass-ceramic

Several glass-ceramic compositions based on lithium silicates have been examined using thermal expansivity, X-ray diffraction, electrical conductivity, electron microscopy and solid state NMR studies. Role of P2O5 in nucleation and of Al2O3 in smoothening expansion behaviour have been particularly highlighted. Magic angle spinning NMR has been used to ascertain presence of Al in tetrahedral positions in the glassy phase

Observations on the role of the steel disc counterface during the sliding of various structural ceramics

Sliding wear characteristics and mechanisms of structural ceramics, namely Al2O3, zirconia-toughened alumina, tetragonal zirconia polycrystals (TZP) and Si3N4 against a steel counterface are influenced by mechanical and tribochemical interactions, specific to the combinations studied. The present paper studies the role of the disc in the sliding wear process of the above ceramics. Experiments were conducted at a pressure of 15.5 MPa between 0.1 and 12.0 m s(-1) with ceramic pins sliding against an EN-24 steel disc. Except in the case of TZP, the disc morphology is sensitive to variations in speed rather than to the pin material. The disc track is (i) mildly abraded at low speeds (about 0.1-0.75 m s(-1)), (ii) severely abraded at intermediate speeds (about 1.0-3.0 m s(-1)), (iii) covered with black patches at high speeds (about 4.0-6.0 m s(-1)) and (iv) completely black at very high speeds (about 7.0-12.0 m s(-1)). In the case of TZP, although black patches appear, transfer of TZP onto the disc surface and high wear of TZP occurs at 4.0 m s(-1). The order of the wear of the disc estimated from profilometric measurements is the same for all the ceramics. Except for Si3N4, the onset of wear of the ceramics is associated with the appearance of deep 'V' grooves on either side of the profile of the disc track. This can be explained on the basis of the thermal and hardness variations. Although other interaction products specific to the ceramic pin are present, the formation of iron oxides dominates the wear of the disc.

Dry sliding wear of Al alloy 2024-Al203 particle metal matrix composites

In the present investigation, Al 2024-15vol.%Al2O3 particulate (average size, 18 mu m) composites were fabricated using the liquid metallurgy route. The wear and friction characteristics of Al alloy 2024 and Al 2024-15vol.%Al2O3p, composite in the as-extruded and peak-aged conditions were studied using a pin-on-disc machine (with a steel disc as the counterface material). The worn surfaces, subsurfaces and the debris were analysed in a scanning electron microscope.The performance of the composite in the as-extruded condition is slightly inferior to that of the unreinforced alloy. However, in the T6 condition, although the wear rates of two materials are initially comparable, the unreinforced alloy seizes while the composite does not within the tested range employed. In the as-extruded condition, the presence of Al2O3 particles is not particularly beneficial as they fracture and result in extensive localized cracking and removal of material from the surface. In the peak-aged condition, however, while the unreinforced alloy exhibits severe plastic deformation and undergoes seizure, there is no significant change in the mechanism in the case of the composite. Except in the case of the peak-aged unreinforced alloy, worn surfaces of all other materials show the presence of an iron-rich layer.

Activities in the spinel solid solution FeXMg1−XAl2O4

Abstract: Activities in the spinel solid solution FexMg1-xAl2O4 saturated with alpha-Al2O3 have been measured for the compositional range 0 < X < 1 between 1100 and 1350 K using a bielectrolyte solid-state galvanic cell, which may be represented as Pt, Fe + FexMg1-xAl2O4 + alpha-Al2O3//(Y2O3)ThO2/ (CaO)ZrO2//Fe + FeAl2O4 + alpha-Al2O3, Pt Activities of ferrous and magnesium aluminates exhibit small negative deviations from Raoult's law. The excess free energy of mixing of the solid solution is a symmetric function of composition and is independent of temperature: Delta G(E) = -1990 X(1 - X J/mol. Theoretical analysis of cation distribution in spinel solid solution also suggests mild negative deviations from ideality. The lattice parameter varies linearly with composition in samples quenched from 1300 K. Phase relations in the FeO-MgO-Al2O3 system at 1300 K are deduced from the results of this study and auxiliary thermodynamic data from the literature. The calculation demonstrates the influence of intracrystalline ion exchange equilibrium between nonequivalent crystallographic sites in the spinel structure on intercrystalline ion exchange equilibrium between the monoxide and spinel solid solutions (tie-lines). The composition dependence of oxygen partial pressure at 1300 K is evaluated for three-phase equilibria involving the solid solutions Fe + FexMg1-xAl2O4 + alpha-Al2O3 and Fe + FeyMg1-yO + FexMg1-xAl2O4. Dependence of X, denoting the composition of the spinel solid solution, on parameter Y, characterizing the composition of the monoxide solid solution with rock salt structure, in phase fields involving the two solid solutions is elucidated. The tie-lines are slightly skewed toward the MgAl2O4 corner.

Metastable phase relations and europium(II) luminescence of barium hexa-aluminates prepared by gel to crystallite conversion

Wet chemical reaction of hydrated alumina gels, Al2O3.yH(2)O(80

Oxide nanotubes prepared using carbon nanotubes as templates

Hollow nanotubes of SiO2, Al2O3, V2O5, and MoO3 have been prepared using carbon nanotubes as templates. The procedure involves coating the carbon nanotubes with tetraethylorthosilicate, aluminum isopropoxide, or vanadium pentoxide gel, followed by calcination and heating at higher temperatures in air to oxidize the carbon. SiO2 nanotubes containing transition metal ions have been prepared by this procedure since such materials may be of use in catalysis.

Preparation of the layered double hydroxide (LDH) LiAl2(OH)(7)center dot 2H(2)O, by gel to crystallite conversion and a hydrothermal method, and its conversion to lithium aluminates

A layered double hydroxide (LDH) with chemical composition LiAl2(OH)(7) . 2H(2)O was prepared via a wet chemical route of gel to crystallite (G-C) conversion at 80 degrees C involving the reaction of hydrated alumina gel, Al2O3.yH(2)O (80 < y < 120) with LiOH (Li2O/Al2O3 greater than or equal to 0.5) in presence of hydrophilic solvents such as ethanol under refluxing conditions. The hydrothermal synthesis was carried out using the same reactants by heating to less than or equal to 140 degrees C in a Teflon-lined autoclave under autogenerated pressure (less than or equal to 20 MPa). Transmission electron microscopy showed needle-shaped aggregates of size 0.04-0.1 mu m for the gel to crystallite conversion product, whereas the hydrothermal products consisted of individual lamellar crystallites of size 0.2-0.5 mu m with hexagonal morphology. The LDH prepared through the gel to crystallite conversion could be converted into LiAl(OH)(4) . H2O or LiAl(OH)(3)NO3 . H2O by imbibition of LiOH or LiNO3, respectively, under hydrothermal conditions. Thermal decomposition of LDH above 1400 degrees C gave rise to LiAl5O8 accompanied by the evaporation of Li2O. LiAl(OH)(4) . H2O and LiAl(OH)(3)NO3 . H2O decomposed in the temperature range 400-1000 degrees C to alpha- or beta-LiAlO2. The compositional dependence of the product, the intermediate phases formed during the heat treatment and the possible reactions involved are described in detail.

The two-step positive temperature coefficient in resistance characteristics of n-(Ba,Pb)TiO3 ceramics created through inclusion of grain boundary modifier additives

Donor-doped n-(Ba,Pb)TiO3 polycrystalline ceramics exhibit distinctly two-step positive temperature coefficient of resistance (PTCR) characteristics when formulated with suitable combinations of B2O3 and Al2O3 as grain boundary modifiers by heterogeneous addition. B2O3 or Al2O3 when added singularly resulted in either steep or broad PTCR jumps respectively across the phase transition. The two-step PTCR is attributed to the activation of the acceptor states, created through B2O3 and Al2O3, for various temperature regimes above the Curie point (T-c). The changing pattern of trap states is evident from the presence of Ti4+-O--Al3+ type hole centres in the grain boundary layer regions, identified in the electron paramagnetic resonance (EPR) spectra. That charge redistribution occurs among the inter-band gap defect states on crossing the Curie temperature is substantiated by the temperature coefficient in the EPR results. Capacitance-voltage results clearly show that there is an increase in the density of trap states with the addition of B2O3 and Al2O3. The spread in energy values of these trap states is evident from the large change in barrier height (phi similar or equal to 0.25-0.6 eV) between 500 and 650 K.

Thiophene adsorption studies on clean and hydrogen-preadsorbed MoS2(100) surface

It is known from temperature-programmed desorption studies that the binding energy of thiophene over Mo/gamma-Al2O3 and Co-Mo/gamma-Al2O3, hydrodesulfurization catalysts, is lower in the presence of hydrogen. The adsorption of thiophene on clean and hydrogen-adsorbed MoS2 was modelled using extended Huckel tight binding band structure calculations. In the eta(1) adsorption configuration the calculations show a lower binding energy for adsorption on the hydrogen-preadsorbed surface similar to that observed experimentally. The lowering is due to an increased occupancy of the Mo density of states in the presence of hydrogen.

Characterization and catalytic properties of combustion synthesized Au/CeO2 catalyst

Ceria-supported Au catalyst has been synthesized by the solution combustion method for the first time and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Au is dispersed as Au as well as Au3+ states on CeO2 surface of 20-30 nm crystallites. On heating the as-prepared 1% Au/CeO2 in air, the concentration of Au3- ions on CeO2 increases at the expense of Au. Catalytic activities for CO and hydrocarbon oxidation and NO reduction over the as-prepared and the heat-treated 1% Au/CeO2 have been carried out using a temperature-programmed reaction technique in a packed bed tubular reactor. The results are compared with nano-sized Au metal particles dispersed on alpha-Al2O3 substrate prepared by the same method. All the reactions over heat-treated Au/CeO2 occur at lower temperature in comparison with the as-prepared Au/CeO2 and Au/Al2O3. The rate of NO + CO reaction over as-prepared and heat-treated 1% Au/CeO2 are 28.3 and 54.0 mumol g(-1) s(-1) at 250 and 300 degreesC respeceively. Activation energy (E,) values are 106 and 90 kJ mol(-1) for CO + O-2 reaction respectively over as-prepared and heat-treated 1% Au/CeO2 respectively.

MOCVD of aluminium oxide films using aluminiurn beta-diketonates as precursors

Deposition of Al2O3 coatings by CVD is of importance because they are often used as abrading material in cemented carbide cutting tools. The conventionally used CVD process for Al2O3 involves the corrosive reactant AlCl3. In this paper, we report on the thermal characterisation of the metalorganic precursors namely aluminium tristetramethyl-heptanedionate [Al(thd)(3)] and aluminium tris-acetylacetonate [Al(acac)(3)] and their application to the CVD of Al2O3 films. Crystalline Al2O3 films were deposited by MOCVD at low temperatures by the pyrolysis of Al(thd)(3) and Al(acac)(3). The films were deposited on a TiN-coated tungsten carbide (TiN/WC) and Si(100) substrates in the temperature range 500-1100degreesC. The as-deposited films were characterised by x-ray diffraction, optical microscopy, scanning and transmission electron microscopy, Auger electron spectroscopy. The observed crystallinity of films grown at low temperatures, their microstructure, and composition may be interpreted in terms of a growth process that involves the melting of the metalorganic precursor on the hot growth surface.

The production of AlN-rich matrix composites by the reactive infiltration of Al alloys in nitrogen

Aluminium nitride (AlN)-Al matrices reinforced with Al2O3 particulate have been fabricated by reactive infiltration of Al-2% Mg alloy into Al2O3 preforms in N-2 in the temperature range of 900-1075 degreesC. The growth of composites of useful thickness was facilitated by the presence of a Mg-rich external getter, in the absence of which composite growth is self-limiting and terminates prematurely. Successful growth of composites has been attributed to the reduction in residual oxygen partial pressure brought about by the reaction with oxygen of highly volatile Mg in the getter alloy. The microstructure of the matrix consists of AlN-rich regions contiguous with the particulate with metal-rich channels in-between, thereby suggesting that nitridation initiates by preferential wicking of alloy along the particle surfaces. The increase in nitride content of the matrix with temperature is consistent with hardness values that vary between similar to3 and 10 GPa. (C) 2002 Acta Materialia Inc. Published by Elsevier Science Ltd. All rights reserved.

Preparation of β-SiAION from silica-alumina gel

Amorphous aluminosilicate gel powders have been subjected to carbothermal reduction and nitridation reaction at high temperature (1673 K). The influence of Al2O3 content in the gel powder on the nature and structure of the product phases has been examined. Between 5% and 9% Al2O3 in the gel powder, it is found that only β-SiAION is formed as the product of CTR/N reaction.