Synthesis and characterization of molybdenum disulphide formed from ammonium tetrathiomolybdate

An investigation has been carried out into the possibility of in situ formation of MoS2 within porous anodic films on aluminium, to improve subsequent tribological behaviour, by re-anodizing in thiomolybdate electrolyte. Acidification of thiomolybdate was employed to simulate the conditions for formation of the sulphide at the anodic film/electrolyte interface, followed by appropriate vacuum heat treatments to study possible temperature effects on the sulphide due to either friction or Joule heating during anodizing. The products of both acidification and heat treatment, characterized by X-ray powder diffraction and scanning electron microscopy, were compared with those formed by direct thermal decomposition of ammonium tetrathiomolybdate crystals. The precipitate formed by acidification was mainly amorphous molybdenum trisulphide (MoS3), which on heat treatment at 450 and 850°C yielded 3R-MoS2. 3R-MoS2 also formed by the thermal decomposition of thiomolybdate crystals. Thermogravimetric and differential thermal analyses showed that the decomposition of MoS3 to MoS2 occurred in the range 220–370°C and revealed the sequence of reaction steps. The findings suggest that mainly amorphous MoS3 is formed as a consequence of changes in the pH of the film/electrolyte interface during re-anodizing but the product is relatively easily transformed to crystalline MoS2 on moderate heating which may occur during wear processes.     

Selective catalytic reduction of NOx by hydrocarbons on Pt/Al2O3 catalysts at low temperatures without the formation of N2O

The selective reduction of nitrogen oxides by hydrocarbons on a Pt catalyst has been investigated. Some variations are observed between different reductants. However, the most significant result is the observation that no N₂O is observed as a by-product when toluene is used as a reductant.     

Reactivity of steam in exhaust gas catalysis III. Steam and oxygen/steam conversions of propane on a Pd/Al2O3 catalyst

A 1% Pd catalyst (38% dispersion) was prepared by impregnating a γ-alumina with palladium acetylacetonate dissolved in acetone. The behaviour of this catalyst in oxidation and steam reforming (SR) of propane was investigated. Temperature-programmed reactions of C₃H₈ with O₂ or with O₂ + H₂O were carried out with different stoichiometric ratios S(S =[O₂]/5[C₃H₈]). The conversion profiles of C₃H₈ for the reaction carried out in substoichiometry of O₂ (S < 1) showed two discrete domains of conversion: oxidation at temperatures below 350°C and SR at temperatures above 350°C. The presence of steam in the inlet gases is not necessary for SR to occur: there is sufficient water produced in the oxidation to form H₂ and carbon oxides by this reaction. Contrary to what was observed with Pt, an apparent deactivation between 310 and 385°C could be observed with Pd in oxidation. This is due to a reduction of PdO_x into Pd⁰, which is much less active than the oxide in propane oxidation. Steam added to the reactants inhibits oxidation while it prevents the reduction of PdO_x into Pd⁰. Compared to Pt and to Rh, Pd has a higher thermal resistance: no deactivation occurred after treatment up to 700°C and limited deactivation after treatment up to 900°C, provided that the catalyst is maintained in an oxygen-rich atmosphere during the cooling.     

Erbium-doped silicon and porous silicon for optoelectronics

Silicon forms the backbone of the microelectronics industry, and possibly, of the optoelectronics industry, hitherto dominated by III/V materials. One of the remaining goals is to build an optical source in silicon. Erbium exhibits luminescent 1.54 μm intra-4f transitions in both silicon and porous silicon. This paper reviews the work which has been carried out in this field and discusses some possible additional applications of erbium-doped silicon in optoelectronics, such as a novel on-chip temperature sensor.     

Oxygen absorption kinetics in YBa2Cu3Ox

The oxygen absorption process in highly aligned YBa₂Cu₃O_x samples in air and in pure oxygen was studied at several constant temperatures. The process can be expressed in two steps, a chemical reaction controlled step and a diffusion controlled step. The kinetic equations are as follows respectively:

(1 − a_t) ln(1 − a_t) + a_t = k_Dt

The activation energy was calculated using an Arrhenius equation. The technical conditions of heat treatment for oxygen absorption of highly aligned YBa₂Cu₃O_x crystals are discussed.     

Optimum design for buckling of plain and stiffened composite axisymmetric shell panels/shells

The buckling of plain and discretely stiffened composite axisymmetric shell panels/shells made of repeated sublaminate construction is studied using the finite element method. In repeated sublaminate construction, a full laminate is obtained by repeating a basic sublaminate, which has a smaller number of plies. The optimum design for buckling is obtained by determining the layup sequence of the plies in the sublaminate by ranking, so as to achieve maximum buckling load for a specified thickness. For this purpose, a four-noded 48-dof quadrilateral composite thin shell element, together with fully compatible two-noded 16-dof composite meridional and parallel circle stiffener elements are used.     

Measurements of distribution of self-bias potential on an RF-plane electrode in plasma etching devices

The self-bias potential (V_dc) induced on an RF-powdered electrode (153 mm Ø) in a plasma is measured using electrical probes which are buried in, de-insulated from, and RF-connected to the electrode. The configuration of the probes allows to study the distribution of V_dc discretely on the electrode. The potential is homogeneous in the absence of external magnetic field. In the presence of a homogeneous magnetic field parallel to the electrode, it is reduced and a monotonous gradient takes place in its distribution due to the plasma shift induced by E × B drift. When the magnetic field is rotated along the axis of the RF-electrode at a frequency less than 50 Hz, the distribution, which is almost identical to the one in a static field, rotates with the magnetic field. On the coordinate system rotating with the magnetic field, the probes are regarded to be rotating. The potential distribution is obtained as a continuous function of the azimuthal angle. Thus the rotation of the field provides information for the experimental interpolation.     

Determining elasticity and strength characteristics of powder coating

Methods are described for forming coating specimens and testing them in pure bending. The proposed tester gives adequate accuracy in determining the elastic characteristics and strength for thin specimens (up to 0.1 mm) of brittle materials of powder-coating type.Translated from Problemy Prochnosti, No. 3, pp. 94–97, March, 1993.     

Instron texture profile of buffalo milk cheddar cheese as influenced by composition and ripening changes

Buffalo milk Cheddar cheese samples of different ages were analysed for compositional attributes (CA), ripening indices (RI) and Instron Textural Profile (ITP). All samples were compositionally alike, except for pH and salt-in-moisture (SM) contents. RI showed significant variations. CA and RI showed highly significant correlations within themselves and with each other, except for moisture with pH, SM with moisture, MNFS, Fat and FDM and Fat with MNFS. The ITPs of cheeses showed significant variations and had highly significant intercorrelations indicating their interdependence. CA (except moisture and MNFS) and RI showed a highly significant correlationship with ITPs. Moisture content showed a highly significant correlationship with all ITPs, except cohesiveness and springiness, where it was significant. MNFS content showed significant correlations only with hardness and brittleness. Stepwise regression analysis revealed that MI was the most predominant factor influencing cheese texture, followed by pH, SM, FDM and TVFA. Knowing Ca and RI, the textural properties of cheeses can be forecast through mathematical equations. Similarly the age of cheese can also be predicted if RI and/or textural properties are known.     

Aromatic nitrations by mixed acid. Slow liquid-liquid reaction regime

Aromatic nitrations by mixed acid have been selected as a specific case of a heterogeneous liquid-liquid reaction. An extensive experimental programme has been followed using adiabatic and heat-flow calorimetry and pilot reactor experiments, supported by chemical analysis. A series of nitration experiments has been carried out to study the influences of different initial and operating conditions such as temperature, stirring speed and sulphuric acid concentration. In parallel, a mathematical model to predict the overall conversion rate has been developed. In this paper the mathematical modelling and the implementation and experimental validation for benzene, toluene and chlorobenzene mononitration in the kinetic control regime (slow liquid-liquid reaction) are presented and discussed.