• S Dash

      Articles written in Bulletin of Materials Science

    • 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.

    • 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

      More Details Abstract Fulltext PDF

      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.

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