Low temperature molten-salt synthesis of nanocrystalline cubic Sr2SbMnO6

Sr2SbMnO6 (SSM) powders were successfully synthesized at reasonably low temperatures via molten-salt synthesis (MSS) method using eutectic composition of 0.635 Li2SO4-0.365 Na2SO4 (flux). High-temperature cubic phase SSM was stabilized at room temperature by calcining the as-synthesized powders at 900 degrees C/10 h. The phase formation and morphology of these powders were characterized via X-ray powder diffraction and scanning electron microscopy, respectively. The SSM phase formation associated with similar to 60 nm sized crystallites was also confirmed by transmission electron microscopy. The activation energy associated with the particle growth was found to be 95 +/- 5 kJ mol(-1). The dielectric constant of the tetragonal phase of the ceramic (fabricated using this cubic phase powder) with and without the flux (sulphates) has been monitored as a function of frequency (100 Hz-1 MHz) at room temperature. Internal barrier layer capacitance (IBLC) model was invoked to rationalize the dielectric properties.

The influence of oxygen impurities on the formation of AlN-Al composites by infiltration of molten Al-Mg

The influence of residual oxygen in nitrogen on the formation of AlN-Al matrix by reactive infiltration has been investigated. Increasing the oxygen content from 10 ppm upwards decreased the nitride content in the matrix from 64 to 6%, Based on the analysis of the availability of oxygen at the Al-melt/gas interface, three distinct scenarios have been proposed (i) at lowest values, oxygen does not interfere with either infiltration or nitridation reaction; (ii) at intermediate values, nitridation is suppressed, however infiltration continues; and (iii) at a critical upper value, the melt passivates without any infiltration. This phenomenon offers control of the AlN/Al ratio in the matrix and the possibility of creation of microstructural gradierits by the appropriate choice of gas mixtures. (C) 2002 Elsevier Science B.V. All rights reserved.

Electrochemical Properties of Li3N Dissolved in Molten LiCl at 900 K

Thermodynamic properties of Li3N dissolved in the molten LiCl salt at 900 K were explored using electrochemical methods. It was difficult to determine precisely the decomposition voltage of Li3N dissolved in the molten salt by cyclic voltammetry. The oxidation wave of N3– ion could not be located with high accuracy. However, the lithium activity of the Pb-Li alloy in equilibrium with the molten salt containing dissolved Li3N under nitrogen atmosphere could be measured electrochemically with high accuracy using the Li/Li + reference electrode. Under the conditions used in this study, the potential of the Li-Pb electrode is equal to the decomposition voltage of Li3N. The activity of Li3N in molten LiCl was determined for anionic fractions of N3– ranging from xN3– = 10–4 to 0.028. The nitride ion concentration in the salt was determined by chemical titration. The activity coefficient of the Li3N at high dilution was found to be very low, around 10–4. The activity coefficient increases sharply with composition and has a value of 0.25 at xN3– = 0.028. ©2001 The Electrochemical Society. All rights reserved.

Thermodynamic properties of Ln-O (Ln = La, Pr, Nd) solid solutions and their deoxidation by molten salt electrolysis

The lanthanide metals lanthanum, praseodymium and neodymium containing 2,200, 2,600, 1,850 mass ppm oxygen, respectively, were deoxidized to 20-30 ppm level at 1,073 K by an electrochemical method. The metal to be deoxidized was used as the cathode in an electrolysis cell which consisted of a graphite anode and molten CaCl2 electrolyte. The calcium metal produced at the cathode by electrolysis effectively deoxidized the lanthanide metal. Calcium oxide produced by deoxidation, dissolved in the melt. The liberation of carbon monoxide/dioxide at the anode was found to prevent accumulation of oxygen in the melt. For a quantitative discussion of the limits of deoxidation achievable by this technique, a thermodynamic investigation of the lanthanide-oxygen (Ln-O ; Ln = La, Pr, Nd) solid solutions was conducted. The lanthanide metal, yttrium and titanium samples were immersed in calcium-saturated CaCl2 melt, containing a small quantity of dissolved CaO, at 1,093 K. The oxygen potential of the melt and the Ln-O solid solutions were obtained from the oxygen content of yttrium samples at equilibrium, and the known thermodynamic properties of yttrium-oxygen solid solution. The results were confirmed by using Y/Y2O3 equilibrium to control the oxygen potential of the molten salt reservoir. The oxygen affinity of the metals was found to decrease in the order : Y > Ti > Nd > Pr > La. The deoxidation results are consistent with the thermodynamic properties of the RE-O solid solutions.

Influence of Bottom Bubbling Rate on Formation of Metal Emulsion in Al-Cu Alloy and Molten Salt System

In steel refining process, an increase of interfacial area between the metal and slag through the metal droplets emulsified into the slag, so-called ``metal emulsion'', is one prevailing view for improving the reaction rate. The formation of metal emulsion was experimentally evaluated using Al-Cu alloy as metal phase and chloride salt as slag phase under the bottom bubbling condition. Samples were collected from the center of the salt phase in the container. Large number of metal droplets were separated from the salt by dissolving it into water. The number, surface area, and weight of the droplets increased with the gas flow rate and have local maximum values. The formation and sedimentation rates of metal droplets were estimated using a mathematical model. The formation rate increased with the gas flow rate and has a local maximum value as a function of gas flow rate, while the sedimentation rate is independent of the gas flow rate under the bottom bubbling condition. Three types of formation mode of metal emulsion, which occurred by the rupture of metal film around the bubble, were observed using high speed camera. During the process, an elongated column covered with metal film was observed with the increasing gas flow rate. This elongated column sometimes reached to the top surface of the salt phase. In this case, it is considered that fine droplets were not formed and in consequence, the weight of metal emulsion decreased at higher gas flow rate.

Polymer-Derived In-Situ Metal Matrix Composites Created by Direct Injection of a Liquid Polymer into Molten Magnesium

We show that a liquid organic precursor can be injected directly into molten magnesium to produce nanoscale ceramic dispersions within the melt. The castings made in this way possess good resistance to tensile deformation at 673 K (400 degrees C), confirming the non-coarsening nature of these dispersions. Direct liquid injection into molten metals is a significant step toward inserting different chemistries of liquid precursors to generate a variety of polymer-derived metal matrix composites. (C) The Minerals, Metals & Materials Society and ASM International 2013

Studies on elastic coupling parameters of fracture modes in orthotropic materials

The characterisation of cracks is usually done using the well known three basic fracture modes, namely opening, shearing and tearing modes. In isotropic materials these modes are uncoupled and provide a convenient way to define the fracture parameters. It is well known that these fracture modes are coupled in anisotropic materials. In the case of orthotropic materials also, coupling exists between the fracture modes, unless the crack plane coincides with one of the axes of orthotropy. The strength of coupling depends upon the orientation of the axes of orthotropy with respect to the crack plane and so the energy release rate components associated with each of the modes vary with crack orientation. The variation, of these energy release rate components with the crack orientation with respect to orthotropic axes, is analyzed in this paper. Results indicate that in addition to the orthotropic planes there exists other planes with reference to which fracture modes are uncoupled.

An Investigation of Friction During Friction Stir Welding of Metallic Materials

The technique of friction stir welding (FSW) puts effective use frictional heat for the purpose of joining metallic materials. In this research article, we present and discuss an experimental method to determine the coefficient of friction during FSW. The experiments were conducted to study the interaction between the FSW tool (a die steel) and the base metal (a high strength aluminum alloy) at various contact pressures (13MPa, 26MPa, and 39MPa) and rotation speeds (200rpm, 600rpm, 1000rpm, and 1400rpm). The experimental results, the microstructure, and the process temperature reveal the experimental setup to be capable of simulating the conditions during FSW. The coefficient of friction was found to vary from 0.15 to 1.4, and the temperature increased to as high as 450C. The coefficient of friction was found to increase with temperature. There exists a critical temperature at which point a steep increase in the coefficient of friction was observed. The critical temperature decreases from 250C at a contact pressure of 26MPa to 200C at contact pressure of 34MPa. Below the critical temperature at a specific contact pressure the maximum coefficient of friction is 0.6, and above the critical temperature it reaches a value as high as 1.4. The steep increase in the coefficient of friction is found to be due to the seizure phenomenon and the contact condition during FSW between the tool and the workpiece (base metal) is found to be sticking.

Einstein Relation in n-Channel Inversion Layers of Nonlinear Optical, Optoelectronic and Related Materials: Simplified Theory, Relative Comparison and Suggestion for an Experimental Determination

In this paper, we study the Einstein relation for the diffusivity to mobility ratio (DMR) in n-channel inversion layers of non-linear optical materials on the basis of a newly formulated electron dispersion relation by considering their special properties within the frame work of k.p formalism. The results for the n-channel inversion layers of III-V, ternary and quaternary materials form a special case of our generalized analysis. The DMR for n-channel inversion layers of II-VI, IV-VI and stressed materials has been investigated by formulating the respective 2D electron dispersion laws. It has been found, taking n-channel inversion layers of CdGeAs2, Cd(3)AS(2), InAs, InSb, Hg1-xCdxTe, In1-xGaxAsyP1-y lattice matched to InP, CdS, PbTe, PbSnTe, Pb1-xSnxSe and stressed InSb as examples, that the DMR increases with the increasing surface electric field with different numerical values and the nature of the variations are totally band structure dependent. The well-known expression of the DMR for wide gap materials has been obtained as a special case under certain limiting conditions and this compatibility is an indirect test for our generalized formalism. Besides, an experimental method of determining the 2D DMR for n-channel inversion layers having arbitrary dispersion laws has been suggested.

Use of microwaves for the synthesis and processing of materials

An overview of the synthesis of materials under microwave irradiation has been presented based on the work performed recently. A variety of reactions such as direct combination, carbothermal reduction, carbidation and nitridation have been described. Examples of microwave preparation of glasses are also presented. Great advantages of fast, clean and reduced reaction temperature of microwave methods are emphasized. The example of ZrO2-CeO2 ceramics has been used show the extraordinarily fast and effective sintering which occurs in microwave irradiation.

In search of inorganic nonlinear optical materials for second harmonic generation

In a search for inorganic oxide materials showing second-order nonlinear optical (NLO) susceptibility, we investigated several berates, silicates, and a phosphate containing trans-connected MO6, octahedral chains or MO5 square pyramids, where, M = d(0): Ti(IV), Nb(V), or Ta(V), Our investigations identified two new NLO structures: batisite, Na2Ba(TiO)(2)Si4O12, containing trans-connected TiO5 octahedral chains, and fresnoite, Ba2TiOSi2O7, containing square-pyramidal TiO5. Investigation of two other materials containing square-pyramidal TiO5 viz,, Cs2TiOP2O7 and Na4Ti2Si8O22. 4H(2)O, revealed that isolated TiO5, square pyramids alone do not cause a second harmonic generation (SHG) response; rather, the orientation of TiO5 units to produce -Ti-O-Ti-O- chains with alternating long and short Ti-O distances in the fresnoite structure is most likely the origin of a strong SHG response in fresnoite,

Nanocrystalline Janus films of inorganic materials prepared at the liquid-liquid interface

The interface between toluene and water has been employed to prepare ultrathin Janus nanocrystalline films of metal oxides, metal chalcogenides and gold, wherein the surface on the organic-side is hydrophobic and the aqueous-side is hydrophilic. We have changed the nature of the metal precursor or capping agent in the organic layer to increase the hydrophobicity. The strategy employed for this purpose is to increase the length of the alkane chain in the precursor or use a perfluroalkane derivative as precursor or as a capping agent. The hydrophobicity and hydrophilicity of the Janus films have been determined by contact angle measurements. The morphology of hydrophobic and hydrophilic sides of the film have been examined by field emission scanning electron microscopy.

Analysis Of Curved Laminated Beams Of Bimodulus Composite-Materials

Composite materials exhibiting different moduli in tension and in compression, commonly called as bimodular composites are being used in many engineering fields. A finite element analysis is carried out for small deflection static behavior of laminated curved beams of bi modulus materials for both solid and hollow circular cross-sections using an iterative procedure. The finite element has 16 d.o.f. and uses the displacement field in terms of first order Hermite in terpolation polynomials. The neutral surface, i.e. the locus of points having zero axial strain is found to vary drastically depending on the loading, lay up schemes and radius of curvature. As il lustrations, plots of the cross-sections of the ruled neutral-surface are presented for some of the investigated cases. Using this element a few problems of curved laminated beams of bimodulus materials are solved for both solid and hollow circular cross-sections.

Initiation Reactions in Thermal Polymerization of Vinyl Monomers in the Molten State

Evidence of the initiation process during uncatalyzed thermal polymerization of vinyl monomers is presented. DSC studies reveal a prominent endothermic effect just before the polymerization exotherm, which is substantiated by the identification of the free radicals produced in the initiation by a quick quenching technique and subsequent detection by ESR at low temperatures.