• Issue front cover thumbnail

      Volume 23, Issue 4

      August 2000,   pages  239-340

    • Phase transitions in Na2TeO4 ceramics

      N K Singh R N P Choudhary

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      Polycrystalline samples of NaTeO4 were prepared by conventional solid-state reaction technique at low temperature (600° C). X-ray powder diffraction (XRD) technique was used to check the formation of single phase NaTeO4 compound with cell parametersa = 10·602(1) åb = 70·622(1) å andc = 8·506(1) å in orthorhombic crystal system. Detailed studies of dielectric constant (ε) (and loss tangent (tan δ) as a function of frequency (400 Hz-10 kHz) and temperature (−120°C–260°C) show that the compound has two phase transitions in the ferroelectric phase.

    • Ceramic joining through reactive wetting of alumina with calcium aluminate refractory cements

      K Geetha A M Umarji T R N Kutty

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      Compositions in CaO-Al2O3 system have been prepared by gel-to-crystallite conversion method. Reactive powders of 1 : 2, 1 : 1, 2 : 1 and 3 : 1 of CaO and2O3 compositions were obtained by calcining the product at 800–1200°C. Fine grained powders were used as refractory cement for joining alumina ceramics. An optimum temperature of 1450°C for 4 h produced joints of satisfactory strength. The microstructure and X-ray phase analysis of the fractured joint surface clearly indicate reactive wetting of the alumina ceramics. This wetting enhances the joining of alumina substrates and can be attributed to the formation of Ca12Al14O33 liquid phase. The results are explained by using CaO-Al2O3 phase diagram.

    • Optimization of time-temperature schedule for nitridation of silicon compact on the basis of silicon and nitrogen reaction kinetics

      J Rakshit P K Das

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      A time-temperature schedule for formation of silicon-nitride by direct nitridation of silicon compact was optimized by kinetic study of the reaction, 3Si + 2N2 = Si3N4 at four different temperatures (1250°C, 1300°C, 1350°C and 1400°C). From kinetic study, three different temperature schedules were selected each of duration 20 h in the temperature range 1250°-1450°C, for complete nitridation. Theoretically full nitridation (100% i.e. 66.7% weight gain) was not achieved in the product having no unreacted silicon in the matrix, because impurities in Si powder and loss of material during nitridation would result in 5–10% reduction of weight gain.

      Green compact of density < 66% was fully nitrided by any one of the three schedules. For compact of density > 66%, the nitridation schedule was maneuvered for complete nitridation. Iron promotes nitridation reaction. Higher weight loss during nitridation of iron doped compact is the main cause of lower nitridation gain compared to undoped compact in the same firing schedule. Iron also enhances the amount of Β-Si3N4 phase by formation of low melting FeSix phase.

    • Phase analysis and dielectric properties of ceramics in PbO-MgO-ZnO-Nb2O5 system: A comparative study of materials obtained by ceramic and molten salt synthesis routes

      M Thirumal A K Ganguli

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      Compositions of the type 3PbO-MgO/ZnO-Nb2O5 were synthesized by the ceramic route at 1000°C and sintered at 1200°C. Powder X-ray diffraction studies of the 1000°C heated products show the presence of the cubic pyrochlore and the columbite (Mg/ZnNb2O6) type phase in the ratio of 3 : 1 for all possible combinations of MgO and ZnO. Further heating at 1200°C led to a decrease in the cubic pyrochlore phase and an increase in the columbite phase by around 10%. Compacted pellets sintered further showed the appearance of the perovskite phase. Similar compositions synthesized using the KCl-NaCl molten salt method at 900°C for 6 h gave a significant amount of the cubic perovskite related phase of the type Pb(Mg/Zn)1/3Nb2/3O3 for all compositions containing MgO. The amount of the perovskite phase was nearly 55% for the Mg rich compositions and decreased with increase in Zn content, the pure Zn composition yielding mainly the cubic pyrochlore phase. On sintering these phases at 1000°C the perovskite phase content decreased. The dielectric constant of the composite materials formed by the ceramic route was in the region of 14 to 20 and varied little with frequency. The composites obtained by the molten salt method, however, showed much larger dielectric constants in the region 40–150 at 500 kHz for various compositions. The dielectric loss tangent of these composites were lower by an order (0.005–0.03 at 500 kHz) compared to the ceramic route.

    • Incorporation of cobalt and nickel metal nano-particles in nano-grain zirconia film matrix by solution route

      S Jana P K Biswas

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      Precursor solutions of cobalt/nickel incorporated nano-grain zirconia films were prepared from aquo-organic solutions of zirconium oxychloride octahydrate and corresponding transition metal nitrate. The films were deposited onto silica glass substrate by the dipping technique. Annealing was made at different temperatures from 450°C to 1200°C ± 5°C in air atmosphere. The range of thickness of the films baked at 450°C was 1800–1870 å. For cobalt system Co3O4 was formed initially at 450°C which gradually transformed to alpha cobalt and next to cubic cobalt along with a non-stoichiometric compound (Zr0.71Co0.23O0.06) with increasing annealing temperature. On the other hand, for nickel system nickel metal of nano-size was observed in the nano-grain zirconia film matrix at 450°C. By increasing annealing temperature to 1200°C, a compound, ZrNi4O, was formed which was found to be stable for ∼ 30 days.

    • Specific heat studies in Ho-Ba-CuO superconductors: Fermionic and bosonic contributions

      Dinesh Varshney Sanjay Shah R K Singh

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      The specific heats of superconducting HoBa2Cu3O7-δ (Tc≅ 92 K) have been theoretically investigated in the temperature domain 70 ≤T ≤110 K. The bosonic (phonons) contribution to the specific heat is estimated from Debye model in the harmonic approximation for high temperature expansion (T > θD/2π) using the moments of the phonon density of states. The fermionic constituent as the electronic specific heat is deduced using a suitable trial function above and belowTc. As a next step the contribution of specific heat by charge oscillations (plasmons) are obtained. The theoretical results from bosonic and fermionic terms are then compared with the experimental results. We find that the specific heats from electronic as well as plasmon term are only a fraction of lattice specific heat and in particular, plasmons do not influence the thermal conduction significantly. The implications of the above analysis are discussed.

    • Conductivity, dielectric behaviour and magnetoelectric effect in copper ferrite-barium titanate composites

      R P Mahajan K K Patankar M B Kothale S A Patil

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      Composites of CuFe2O4 and BaTiO3 were prepared using a conventional ceramic double sintering process. The presence of both phases was confirmed by X-ray diffraction. The variations of resistivity and thermo emf with temperature in these samples were studied. All the composites showed n-type behaviour. The variation of dielectric constant (έ′) in the frequency range 100 Hz to 1 MHz and with temperature at constant frequency were studied. The conduction phenomenon was explained on the basis of a small polaron-hopping model. Also confirmation of this phenomenon was made with the help of a.c. conductivity measurements. The static value of the magnetoelectric conversion factor, i.e. d.c. (ME)H was studied as a function of intensity of the magnetic field. The maximum value of ME coefficient was observed for 75% ferroelectric phase composite.

    • EPR, IR and DC conductivity studies ofxCuO-(100-x) Bi2O3 glasses

      D Sreenivasu V Chandramouli

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      Glass systemxCuO-(100-x) Bi2O3 in the composition range 30–60 mol% of CuO is prepared by melt-quenching technique. The ESR spectra show no hyperfine splittings in parallel part but the peak to peak field width is found to vary with CuO content. The observedg effective values are found to vary with copper oxide. The absence of hyperfine splittings is due to inhomogeneous broadening. The observed IR spectra suggest the presence of Bi-O bonds. The structure is changing from [BiO6] octahedral to [BiO3] pyramidal units with increasing CuO concentration. D.C. electrical conductivity results indicate that the conduction is electron in nature and arises out of adiabatic hopping of polarons. The activation energy is found to be concentration and temperature dependent.

    • Dielectric properties of NaF-B2O3 glasses doped with certain transition metal ions

      M Krishna Murthy K S N Murthy N Veeraiah

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      Dielectric constant ε, loss tan δ, a.c. conductivity Σ and dielectric breakdown strength of NaF-B2O3 glasses doped with certain transition metal ions (viz. Cu2+, VO2+, Ti4+ and Mn4+) are studied in the frequency range 102-107 Hz and in the temperature range 30–250°C. The values of ε, tan δ, Σa.c. are found to be the highest for Cu2+ doped glasses and the lowest for Mn4+ doped glasses. Activation energy for a.c. conduction and the value of dielectric breakdown strength are found to be the lowest for Cu2+ doped glasses and the highest for Mn4+ doped glasses. With the help of infrared spectra, increase in the values of ε and tan δ of these glasses with frequency and temperature are identified with space charge polarization. An attempt has been made to explain a.c. conduction phenomenon on the basis of quantum mechanical tunneling model (QMT)/carrier barrier hopping model.

    • A test for diffusional coherency strain hypothesis in the discontinuous precipitation in Mg-Al alloy

      K T Kashyap C Ramachandra V Bhat B Chatterji

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      Discontinuous precipitation (DP) occurs in many alloy systems under certain conditions. Although solute supersaturation is the chemical driving force for DP, this has to be coupled with another driving force for grain boundary migration. This was identified to be diffusional coherency strain ahead of the moving boundary in the case of diffusion induced grain boundary migration (DIGM) and liquid film migration (LFM). In the present work, the validity of diffusional coherency strain hypothesis is verified in Mg-Al alloy, which exhibits discontinuous precipitation. Samples were tested with an applied stress simultaneously with discontinuous precipitation and it was found that the velocity of the boundaries both parallel and transverse to the stress axis obeys the model for diffusional coherency strain. This work can be used as a conclusive evidence for diffusional coherency strain hypothesis for the occurrence of discontinuous precipitation in Mg-Al alloys.

    • Thermal formation of corundum from aluminium hydroxides prepared from various aluminium salts

      J Temuujin Ts Jadambaa K J D Mackenzie P Angerer F Porte F Riley

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      Aluminium hydroxides have been precipitated from various aluminium salts and the differences in their thermal behaviour have been investigated. Pseudoboehmite derived from the nitrate, sulfate and chloride all form γ-Al2O3 at ∼ 400°C but the formation of α-A12O3 at 1200°C occurs more readily in the material derived from the sulfate. This contains a higher concentration of anionic impurities related to differences in the solubility of the original aluminium salts. The sulfate is retained in the gel to higher temperatures at which its eventual decomposition may lead to the formation of a reactive pore structure which facilitates the nucleation of α-A12O3.

    • Calcium ferrite formation from the thermolysis of calcium tris (maleato) ferrate(III)

      B S Randhawa Kamaljeet Sweety

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      For preparing calcium ferrite, calcium tris (dmaleato) ferrate(III) precursor was prepared by mixing aqueous solutions of iron(III) maleate, calcium maleate and maleic acid. Various physico-chemical techniques i.e. TG, DTG, DTA, Mössbauer, XRD, IR etc have been used to study the decomposition behaviour from ambient to 900°C and ferrite formation. Three consecutive decomposition steps leading to the formation of α-Fe2O3 and calcium carbonate have been observed at various stages of thermolysis. In the final stage the ferrite, bdCa2Fe2O5, is obtained as a result of solid state reaction between α-Fe2O3 and calcium carbonate at 788°C, a temperature much lower than for ceramic method. The results have been compared with those of the oxalate precursor.

    • Gas-chromism in ultrasonic spray pyrolyzed tungsten oxide thin films

      P S Patil

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      A simple and inexpensive ultrasonic spray pyrolysis (USP) technique has been employed to deposit tungsten oxide (WO3) thin films by spraying 2.0 mM aqueous ammonium metatungstate solution onto the amorphous glass substrates kept at 250°C. The films were further annealed at 400°C for 4 h in air. X-ray diffraction (XRD) technique was used to determine the crystallinity and to identify the WO3 phases. It was found that the films were sub-stoichiometric, WO3-z. To study gas-induced properties, a catalyzing layer of platinum (Pt) was sputtered onto it. The gas-induced electrical and optical properties of Pt/WO3/glass samples were studied and results reported. It was found that electrical resistivity decreased by a factor of 10 within 2 min and stabilized after 15 min, after H2 gas exposure. Similarly the optical transmittance of the samples attenuated from 55% to 10% within 15–20 min. The reversible changes in electrical resistivity and optical transmittance were observed when the samples were exposed to oxygen. The response times and sensitivity of the samples were estimated.

    • Structural characterization of vacuum evaporated ZnSe thin films

      Pradip Kr Kalita B K Sarma H L Das

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      Thermally evaporated ZnSe thin films deposited on glass substrates within substrate temperatures (Ts)at 303 K-623 K are of polycrystalline nature having f.c.c. zincblende structure. The most preferential orientation is along [111] direction for all deposited films together with other abundant planes [220] and [311]. The lattice parameter, grain size, average internal stress, microstrain, dislocation density and degree of preferred orientation in the film are calculated and correlated withTs.

    • An experimental investigation of electrical conductivities in biopolymers

      H Mallick A Sarkar

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      Gum arabica obtained from acacia plant is a conducting biopolymer. Experiments are carried out on this natural gum arabica. In the present study TGA, ion transference number, transient ionic current, thermal analysis, frequency and temperature variation of a.c. conductivity, Arrhenius plot and volt-ampere characteristics of specimens are carried out. The total electrical conductivity of these biopolymers are comparable to that of synthetic polymers doped with inorganic salts. The ion transference number of these biopolymers show their superionic nature of electrical conduction. The overall conduction mechanism seems to be protonic in nature rather than electronic one.

    • Electrical transport in ethyl cellulose-chloranil system

      P K Khare R K Pandey P L Jain

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      The charge-transport behaviour in pure and chloranil (Chl) doped ethyl cellulose (EC) system has been studied by measuring the dependence of current on field, temperature, electrode material and dopant concentration. The role of doping molecular concentration in the polymer matrix and modification in the conduction characteristics are studied. Lowering of the activation energy due to doping was observed. The current was found to increase with an increase in the chloranil concentration. An explanation for this has been attempted on the basis of formation of molecular aggregates between chloranil molecules and ethoxy groups of ethyl cellulose. It is suggested that chloranil occupies interstitial positions between the polymer chains and assists in carrier transportation by reducing the hopping barriers. The current-voltage characteristics of different samples are analyzed using space charge limited current theory and quantitative information about the transport parameters is derived. The values of effective drift mobility and trapped charge carrier concentration which result in the build up of space charge have been calculated.

    • Current-voltage studies on β-FeSi2/Si heterojunction

      A Datta S Kal S Basu

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      I-V characteristics of both β-FeSi2/n-Si and β-FeSi2/p-Si were studied at room temperature. The junctions were formed by depositing Fe on Si selectively followed by thermal annealing and some samples were later treated by pulsed laser. Temperature of thermal annealing and diode area were also varied.I-V studies on all these samples were done and ideality factors were computed. Results obtained were interpreted.

    • ]Electrical conductivity measurements on gel grown KDP crystals added with some ammonium compounds

      T H Freeda C Mahadevan

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      Pure and impurity added [with NH4CI, NH4NO3, NH44H2PO4, (NH4)2CO3 and (NH4)2SO4] KDP single crystals were grown by the gel method using silica gels. Electrical conductivity measurements were carried out along both the unique axis and perpendicular directions at various temperatures ranging from 28 to 140°C by the conventional two-probe method. The present study shows that the conductivity in KDP crystals, for all the five dopants considered, increases with the increase in impurity concentration and temperature. Activation energies were also determined and reported.

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