• A K Tyagi

      Articles written in Bulletin of Materials Science

    • Carbonaceous alumina films deposited by MOCVD from aluminium acetylacetonate: a spectroscopic ellipsometry study

      M P Singh G Raghavan A K Tyagi S A Shivashankar

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      Spectroscopic ellipsometry was used to characterize carbonaceous, crystalline aluminium oxide films grown on Si(100) by low-pressure metal organic chemical vapour deposition, using aluminium acetylacetonate as the precursor. The presence of carbon in the films, attribured to the use of a metalorganic precursor for the deposition of films, was identified and analysed by secondary ion mass spectroscopy and X-ray photoelectron sectroscopy, for the elemental distribution and the chemical nature of the carbon in the films, respectively. Ellipsometry measurments over the photon energy range 1.5-5 eV were used to derive the pseudo-dielectric function of the aluminium oxide-containing films. Multi-layer modelling using linear regression techniques and the effective medium approximation were carried out to extract the structural details of the specimens. The excellent fit between the simulated and experimental optical data validates the empirical model for alumina-containing coatings grown by MOCVD.

    • Thermogravimetry-evolved gas analysis–mass spectrometry system for materials research

      M Kamruddin P K Ajikumar S Dash A K Tyagi Baldev Raj

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      Thermal analysis is a widely used analytical technique for materials research. However, thermal analysis with simultaneous evolved gas analysis describes the thermal event more precisely and completely. Among various gas analytical techniques, mass spectrometry has many advantages. Hence, an ultra high vacuum (UHV) compatible mass spectrometry based evolved gas analysis (EGA–MS) system has been developed. This system consists of a measurement chamber housing a mass spectrometer, spinning rotor gauge and vacuum gauges coupled to a high vacuum, high temperature reaction chamber. A commercial thermogravimetric analyser (TGA: TG + DTA) is interfaced to it. Additional mass flow based gas/vapour delivery system and calibration gas inlets have been added to make it a versatile TGA–EGA–MS facility. This system which gives complete information on weight change, heat change, nature and content of evolved gases is being used for

      temperature programmed decomposition (TPD),

      synthesis of nanocrystalline materials,

      gas–solid interactions and

      analysis of gas mixtures.

      The TPD of various inorganic oxyanion solids are studied and reaction intermediates/products are analysed off-line. The dynamic operating conditions are found to yield nanocrystalline products in many cases. This paper essentially describes design features involved in coupling the existing EGA–MS system to TGA, associated fluid handling systems, the system calibration procedures and results on temperature programmed decomposition. In addition, synthesis of a few nanocrystalline oxides by vacuum thermal decomposition, gas analysis and potential use of this facility as controlled atmosphere exposure facility for studying gas–solid interactions are also described.

    • Effect of annealing on magnetic properties and silicide formation at Co/Si interface

      Shivani Agarwal V Ganesan A K Tyagi I P Jain

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      The interaction of Co (30 nm) thin films on Si (100) substrate in UHV using solid state mixing technique has been studied. Cobalt was deposited on silicon substrate using electron beam evaporation at a vacuum of 4 × 10-8 Torr having a deposition rate of about 0.1 Å/s. Reactivity at Co/Si interface is important for the understanding of silicide formation in thin film system. In the present paper, cobalt silicide films were characterized by atomic force microscopy (AFM) and secondary ion mass spectroscopy (SIMS) in terms of the surface and interface morphologies and depth profile, respectively. The roughness of the samples was found to increase up to temperature, 300°C and then decreased with further rise in temperature, which was due to the formation of crystalline CoSi2 phase. The effect of mixing on magnetic properties such as coercivity, remanence etc at interface has been studied using magneto optic Kerr effect (MOKE) techniques at different temperatures. The value of coercivity of pristine sample and 300°C annealed sample was found to be 66 Oe and 40 Oe, respectively, while at high temperature i.e. 748°C, the hysteresis disappears which indicates the formation of CoSi2 compound.

    • Formation of InN nanoparticle and nanorod structures by nitrogen plasma annealing method

      Ajay Kumar Mann Deepak Varandani Bodh Raj Mehta Lalit Kumar Malhotra G Mangamma A K Tyagi

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      In the present study, a novel method involving nitrogen plasma annealing has been reported for preparing InN nanoparticle/nanorod structures and for improving the properties of InN nanoparticle layers. Plasma annealed structures have been characterized by X-ray diffraction, atomic force microscopy and photoluminescence spectroscopy techniques. InN nanoparticle layers have been prepared using activated reactive evaporation set up. It has been observed that there is a remarkable improvement in the conductivity and crystallinity of InN nanoparticle layers on annealing in nitrogen plasma. This has been attributed to the increase in the nitrogen content of the samples. Experiments involving plasma annealing of In nanorods deposited oxide template has also been carried out. It was found that on plasma treatment In nanorods get converted to mixed phase InN nanorods with hexagonal and cubic fractions.

    • Optical and mechanical properties of diamond like carbon films deposited by microwave ECR plasma CVD

      S B Singh M Pandey N Chand A Biswas D Bhattacharya S Dash A K Tyagi R M Dey S K Kulkarni D S Patil

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      Diamond like carbon (DLC) films were deposited on Si (111) substrates by microwave electron cyclotron resonance (ECR) plasma chemical vapour deposition (CVD) process using plasma of argon and methane gases. During deposition, a d.c. self-bias was applied to the substrates by application of 13.56 MHz rf power. DLC films deposited at three different bias voltages (–60 V, –100 V and –150 V) were characterized by FTIR, Raman spectroscopy and spectroscopic ellipsometry to study the variation in the bonding and optical properties of the deposited coatings with process parameters. The mechanical properties such as hardness and elastic modulus were measured by load depth sensing indentation technique. The DLC film deposited at –100 V bias exhibit high hardness (∼ 19 GPa), high elastic modulus (∼ 160 GPa) and high refractive index (∼ 2.16–2.26) as compared to films deposited at –60 V and –150 V substrate bias. This study clearly shows the significance of substrate bias in controlling the optical and mechanical properties of DLC films.

    • Estimation of vapour pressure and partial pressure of subliming compounds by low-pressure thermogravimetry

      G V Kunte Ujwala Ail P K Ajikumar A K Tyagi S A Shivashankar A M Umarji

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      A method for the estimation of vapour pressure and partial pressure of subliming compounds under reduced pressure, using rising temperature thermogravimetry, is described in this paper. The method is based on our recently developed procedure to estimate the vapour pressure from ambient pressure thermogravimetric data using Langmuir equation. Using benzoic acid as the calibration standard, vapour pressure–temperature curves are calculated at 80, 160 and 1000 mbar for salicylic acid and vanadyl bis-2,4-pentanedionate, a precursor used for chemical vapour deposition of vanadium oxides. Using a modification of the Langmuir equation, the partial pressure of these materials at different total pressures is also determined as a function of temperature. Such data can be useful for the deposition of multi-metal oxide thin films or doped thin films by chemical vapour deposition (CVD).

    • Hydrogen absorption/desorption characteristics of room temperature ZrMn2-𝑥Ni𝑥 system (𝑥 = 1.25-1.50)

      Vinod Kumar D Pukazhselvan A K Tyagi S K Singh

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      The present communication deals with the hydrogen storage characteristics of C15 laves phase ZrMn2-𝑥Ni𝑥 system tailored within the x values of 1.25 to 1.50. Drastic variations in thermodynamics of the hydride phase is observed for any little changes of concentration x within this narrow range. The most promising room temperature hydrogen storage materials are found to be formed within the range of 1.35 to 1.45 where ∼ 2.5 to 2.9 H/F.U. can be reversibly stored under the ideal operating conditions. The heat of the reaction is found to be ∼ 17 kJ/mol, which means these are promising candidates for stationary and short range mobile applications. The phase structural features and the thermodynamic aspects of all the materials are discussed in detail.

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