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      Volume 25, Issue 7

      December 2002,   pages  583-676

    • Synthesis and characterization of 𝛽 type solid solution in the binary system of Bi2O3–Eu2O3

      O Turkoglu M Soylak I Belenli

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      We have investigated Bi2O3–Eu2O3 binary system by doping with Eu2O3 in the composition range from 1 to 10 mole% via solid state reactions and succeeded to stabilize 𝛽-Bi2O3 phase which is metastable when pure. Stability of 𝛽-Bi2O3 polymorph was influenced by heat treatment temperature. Tetragonal type solid solution was obtained in 3–6 mole% addition range when annealed at 750°C and the range was 2–7 mole% when annealed at 800°C. We have also carried out investigations on lattice parameters, microstructural properties and elemental compositions of this 𝛽 type solid solution for each doping ratio. Lattice parameters increased with amount of Eu2O3 addition. Our experimental observations strongly suggested that oxygen deficiency type non-stoichiometry is present in doped 𝛽 type solid solutions.

    • Formation of oxygen related donors in step-annealed CZ–silicon

      Vikash Dubey Shyam Singh

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      The effect of step-annealing necessitated by the difficulties being faced in the long duration annealing treatments to be given to CZ–silicon has been studied. One pre-anneal of 10 h followed by annealing of 10 h causes a decrease in the absorption coefficient for carbon (𝛼c). Oxygen and carbon both accelerate thermal donor (TD) formation process but oxygen plays a dominating role. Three anneals of 10 h each followed by one anneal of 10 h support the view that carbon suppresses the donor formation. The absorption coefficient for carbon decreases after a few number of step-anneals resulting in the transformation of TD to new donor (ND) as brought about by annealing at temperature, > 500°C. It is quite logical to conclude that step-annealing may bring about the same results as obtained on continuous annealing for a longer duration.

      The results have been fully supported by proper interpretation in the light of existing theories.

    • Preparation of Si3N4–SiC composites by microwave route

      M Panneerselvam K J Rao

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      Si3N4–SiC composites have been microwave sintered using 𝛽-Si3N4 and 𝛽-SiC as starting materials. Si3N4 rich compositions (95 and 90 vol.% Si3N4) have been sintered above 96% of theoretical density without using any sintering additives in 40 min. A monotonic decrease in relative density is observed with increase in SiC proportion in the composite. Decrease in relative density has manifested in the reduction of fracture toughness and microhardness values of the composite with increase in SiC content although the good sintering of matrix Si3N4 limits the decrease of fracture toughness. Highest value of fracture toughness of 6.1 MPa m1/2 is observed in 10 vol.% SiC composite. Crack propagation appears to be transgranular in the Si3N4 matrix and the toughening of the composites is through crack deflection around hard SiC particles in addition to its debonding from the matrix.

    • Evaluation of a.c. conductivity of rubber ferrite composites from dielectric measurements

      S Sindhu M R Anantharaman Bindu P Thampi K A Malini Philip Kurian

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      The effect of frequency, composition and temperature on the a.c. electrical conductivity were studied for the ceramic, Ni1–𝑥Zn𝑥Fe2O4, as well as the filler (Ni1–𝑥Zn𝑥Fe2O4) incorporated rubber ferrite composites (RFCs). Ni1–𝑥Zn𝑥Fe2O4 (where 𝑥 varies from 0 to 1 in steps of 0.2) were prepared by usual ceramic techniques. They were then incorporated into a butyl rubber matrix according to a specific recipe. The a.c. electrical conductivity (𝜎a.c.) calculations were carried out by using the data available from dielectric measurements and by employing a simple relationship. The a.c. conductivity values were found to be of the order of 10–3 S/m. Analysis of the results shows that 𝜎a.c. increases with increase of frequency and the change is same for both ceramic Ni1–𝑥Zn𝑥Fe2O4 and RFCs. 𝜎a.c. increases initially with the increase of zinc content and then decreases with increase of zinc. Same behaviour is observed for RFCs too. The dependence of 𝜎a.c. on the volume fraction of the magnetic filler was also studied and it was found that the a.c. conductivity of RFCs increases with increase of volume fraction of the magnetic filler. Temperature dependence of conductivity was studied for both ceramic and rubber ferrite composites. Conductivity shows a linear dependence with temperature in the case of ceramic samples.

    • Characterization of silane coated hollow sphere alumina-reinforced ultra high molecular weight polyethylene composite as a possible bone substitute material

      S Roy S Pal

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      Silane coated hollow sphere alumina ceramic particles were moulded with ultra high molecular weight polyethylene (UHMWPE) to form a series of composites with alumina weight percent in the range from 15 to 50. The composites were prepared in a cylindrical mould using powder-processing technique. The composites were characterized for mechanical properties using destructive and non-destructive ultrasonic testing methods. The physical properties of the composite were determined and compared with those of cortical bone.

    • Metal oxalate complexes as novel inorganic dopants: Studies on their effect on conducting polyaniline

      R Murugesan E Subramanian

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      Doped polyaniline materials with metal oxalate complexes of Cr, Fe, Mn, Co and Al were synthesized by in situ chemical oxidative polymerization of aniline using potassium perdisulphate as oxidant in aqueous sulphuric acid medium. These polymer materials were characterized by chemical analyses, spectral studies (UV-visible and IR), X-ray diffraction and thermal techniques and also by conductivity measurements by four-probe technique. The presence of complex anion in polyaniline material was confirmed by chemical and spectral analyses. The yield and conductivity of metal oxalate doped polyanilines were found to be high when compared to the simple sulphate ion doped polyaniline prepared under similar condition. UV-visible and IR spectral features not only confirmed the polyaniline doping by complex anions but also substantiated their facilitating effect on conductivity. The X-ray diffraction patterns indicated some crystalline nature in metal oxalate doped polyaniline and amorphous in polyaniline sulphate salt. The conductivity of the polymer samples strongly depended on the degree of crystallinity induced by complex counter anions as dopant. All the polymer materials, as evident from TGA curves, were observed to undergo three-step degradation of water loss, de-doping and decomposition of polymer. Further, the thermal stability of polyaniline was found to improve on doping with metal oxalate complex.

    • Microstructural characterization of the 𝛾-TiAl alloy samples fabricated by direct laser fabrication rapid prototype technique

      D Srivastava

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      A direct laser fabrication technique (DLF) has been used to fabricate near net shape samples of a 𝛾-TiAl alloy using gas atomized Ti48A148Mn2Nb2 alloy powder as a feed stock material. The microstructures of these Ti48Al48Mn2Nb2 laser treated samples have been characterized using optical, scanning (SEM) and transmission electron microscopy (TEM), both immediately after laser fabrication and after heat treatments. The microstructural studies have shown that the microstructure is heterogeneous in nature and extremely fine in comparison with the conventionally processed material. The process parameters such as laser power and laser scanning speed greatly influence the morphology and the microstructure of the laser treated samples. Heat treatments for a number of process conditions have been carried out to examine the stability of the microstructure which remains stable up to 973 K and rapid grain coarsening occurs at 1273 K. A fully recrystallized and uniform microstructure is obtained after annealing at 1073 K for 24 h and compositional heterogeneity present in the laser-fabricated samples is eliminated. Annealing in the 𝛼 phase field followed by air cooling and annealing in (𝛼2 + 𝛾) phase region gives rise to a homogeneous and uniform microstructure. However, the microstructure is much coarser than the microstructure of the DLF samples.

    • Fine structures in Fe3Al alloy layer of a new hot dip aluminized steel

      Li Yajiang Wang Juan Zhang Yonglan X Holly

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      The fine structure in the Fe–Al alloy layer of a new hot dip aluminized steel (HDA) was examined by means of X-ray diffractometry (XRD), electron diffraction technique, etc. The test results indicated that the Fe–Al alloy layer of the new aluminized steel mainly composed of Fe3Al, FeAl and 𝛼-Fe (Al) solid solution. There was no brittle phase containing higher aluminum content, such as FeAl3 (59.18% Al) and Fe2Al7 (62.93% Al). The tiny cracks and embrittlement, formerly caused by these brittle phases in the conventional aluminum-coated steel, were effectively eliminated. There was no microscopic defect (such as tiny cracks, pores or loose layer) in the coating. This is favourable to resist high temperature oxidation and corrosion of the aluminized steel.

    • Microhardness studies on as-grown faces of NaClO3 and NaBrO3 crystals

      K Kishan Rao V Surender B Saritha Rani

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      Single crystals of NaClO3 and NaBrO3 are grown from their aqueous solutions at a constant temperature of 35°C by slow evaporation by using good quality seed crystals. Systematic microhardness studies are made on as-grown faces of these crystals at various loads. Typical cracks are observed at the corners of the impressions in NaClO3 whereas in addition to the cracks at the corners microcracks also appeared in NaBrO3 crystals around the impressions. The impressions formed in NaBrO3 are not very clear as in NaClO3, a possible mechanism for it is discussed. The work hardening index number (𝑛) for both these crystals is around 1.6 suggesting that these are moderately harder samples. The hardness studies point out that NaBrO3 is harder than NaClO3 (𝛥 𝐻 ≈ 100 kg/mm2), this could be due to strong inter ionic forces acting between Na–Br in NaBrO3 crystals. Using Gilman’s empirical relation, hardness values are calculated from the values of elastic constants (𝐶44) and are found to be close to the experimental results.

    • A simple technique for a.c. conductivity measurements

      R Padma Suvarna K Raghavendra Rao K Subbarangaiah

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      An inexpensive, indigenous and a simple electronic instrument based on voltage follower, current–to–voltage converter, zero crossing detector and a phase detector has been developed for measurement of a.c. conductivity. Real and imaginary parts of complex impedance are determined for a given sample as a function of frequency and the given sample is represented by a pure electronic model.

    • Comparative study of the electronic structure of natural and synthetic rubies using XAFS and EDAX analyses

      P Parikh D M Bhardwaj R P Gupta N L Saini S Fernandes R K Singhal D C Jain K B Garg

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      We have studied the Cr–K-edge XANES and EXAFS in natural Indian rubies from two sources and a synthetic ruby at ESRF. Weight % of various constituents in them is determined using EDAX measurements. Taking the results from the three techniques together we are able to demonstrate their feasibility in quantitative study of precious stones.

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