Naveen V. Kulkarni

A novel approach towards selective bulk synthesis of few-layer graphenes in an electric arc

The paper demonstrates the selective bulk synthesis of few-layer graphenes by optimizing an external magnetic field assisted electric arc. An ultra-high purity glassy graphite anode was sublimated in an argon atmosphere, and carbon nanotubes (CNTs), along with graphene sheets, were found inside the deposit formed on the cathode. Both the high purity CNTs and the graphene sheets, with minimal structural defects, were synthesized separately by varying the strength and orientation of the external magnetic field. The as-synthesized carbonaceous samples were characterized with the help of transmission electron microscopy, selected area electron diffraction (SAED), Raman spectroscopy and thermogravimetry with the objective of optimizing the highest selective production of 2D graphene structures. The as-synthesized graphene sheets exhibited a relatively high degree of graphitization and low structural defect density as confirmed by Raman spectroscopy. They were found to exhibit higher oxidation temperature (767 °C) than that of the carbon nanocrystalline particles (690 °C), as inferred from the thermogravimatric analysis. Moreover, they were found to roll up at their edges on account of their surface energy minimization. This was confirmed by the SAED analysis. With this new technique, we could successfully synthesize 2D graphene structures at the rate of a few g h−1.

In Situ Optical Emission Spectroscopic Investigations During Arc Plasma Synthesis of Iron Oxide Nanoparticles by Thermal Plasma

Investigations using in situ precursor spectroscopy during the growth of nanoparticles of iron oxide by thermal plasma induced gas phase condensation method have been shown to be useful for correlating the size of nanoparticles with existing plasma parameters. The relative abundance of ionized Fe species inside the plasma plume is seen to directly establish the relation between particle size, arc current, arc length, and ambient pressure of the reacting oxygen gas. The argon plasma from a transferred arc reactor is made to impinge on the anode that is allowed to vaporize and react with oxygen. The spectral line profiles of both Ar and Fe along the plasma column during the synthesis of nanoparticles have been proved to be useful in understanding the growth mechanism. Band intensities of FeO molecular states indicated the inverse relation with particle sizes that have been correlated to the two competitive processes in which energy is released, namely: 1) one involving the radiative transition and 2) the other that of the growth by coagulation. Atomic Boltzmann plots are used for estimating the temperatures of the zones, whereas particle sizes have been inferred using transmission electron microscopic measurements

A new approach towards improving the quality and yield of arc-generated carbon nanotubes

The paper reports the deterministic effects of a focusing electric field in improving the purity and yield of the arc-generated carbon nanotubes (CNTs). The method utilizes a focusing electrostatic field, which was superimposed on the arc symmetrically. The focusing voltage was varied from 0 to 1200 V at steps of 200 V and a number of cathode deposits, thus generated, were collected and thoroughly analysed in their totality with the help of weight balance, Raman spectroscopy, transmission electron microscopy and thermogravimetry. With the optimally configured focusing electric field, the arc generator is found to utilize nearly 85% of the consumed anode material, for converting into cathode deposit consisting of CNTs, as compared with about 35% in the conventional arc plasma method. The sample prepared under optimized conditions exhibited high oxidation temperature (851 °C) in the thermogravimetric analysis, negligible D band intensity along with a reduced G band line-width (14 cm−1) in the Raman spectrum, confirming the presence of high purity CNTs with a high relative yield.

In Situ Studies of Emission Characteristics of the DC Thermal Arc Plasma Column During Synthesis of Nano-AlN Particles

The growth process of nanoparticles and nanowires of AlN by thermal-plasma-assisted gas phase condensation reaction has been investigated by optical emission spectroscopy. The concentrations of the reacting precursors in the plasma have been correlated to the crystalline phases of nanoparticles of AlN found from X-ray diffraction analysis. The size and morphology of the nanoparticles have been studied by transmission electron microscope investigations of as-synthesized powder at a set of reactor parameters, which included arc current, reactor pressure, and standoffs of the arc column. An attempt has been made to correlate the growth of AlN to that of the precursor density present in the plasma reaction zone

Role of arc plasma instability on nanosynthesis

Recent studies have shown that use of direct current arc plasma jet is a promising technique for bulk generation of nanostructures. This paper presents a dynamical study on such systems during the synthesis and attempts to correlate the role of inherent arc fluctuations on the properties of nanostructures produced. Different fluctuations detected during the process of nanosynthesis have been characterized in terms of behavior in real time, phase space, frequency space, fractal dimension, Lyapunov exponent of evolution and diagnosed to be chaotic. For the first time, it has been shown that size of nanoparticles are strongly related to the Lyapunov exponent of inherent voltage fluctuations realized during the synthesis. Interesting features of such dependences under different process conditions have been brought out. Since chaotic systems are controllable, the study brings out the possibility of development of new size control strategies for nanosynthesis.

Phase controlled structure formation of the nanocrystalline zirconia using thermal plasma technique

Nanocrystalline ZrO2 powder was synthesized by dc transferred arc thermal plasma reactor by homogeneous gas phase condensation mechanism. ZrO2 is an oxide ceramic with a high melting point, good chemical resistance and high mechanical strength. When doped with certain oxides, ZrO2 shows high ionic conductivity. ZrO2 is also recognized as a superior thermal barrier material. Thermal plasma synthesis of oxide nano materials shows pressure dependent crystalline phase and crystallite size. The X-ray diffraction analysis clearly shows that as the ambient oxygen gas pressure increases from 100 Torr to 1000 Torr the abundance of tetragonal phase goes on increasing. The morphology of the as synthesized ZrO2 powder was found to be spherical and independent on the ambient gas pressure as seen from the Scanning Electron Microscopy studies. The specific surface area of powder was calculated using the nitrogen gas adsorption Brunauer, Emmett, Teller surface area analysis technique and found no much variation.

MICRON-PARTICULATE CRYSTALLINE HEXAGONAL ALUMINIUM NITRIDE: A NOVEL, EFFICIENT AND VERSATILE HETEROGENEOUS CATALYST FOR THE SYNTHESIS OF SOME HETEROCYCLIC COMPOUNDS

The present work reports the application of micron-particulate crystalline hexagonal aluminium nitride/aluminium as a novel, mild acidic and reusable solid heterogeneous catalyst in organic synthesis. The catalyst was synthesized by thermal plasma technique and characterized using X-ray diffractometer and scanning electron microscopy. It catalyzes efficiently many organic transformations such as the synthesis of heterocyclic compounds 2,4,5-triaryl-substituted imidazoles and 2-aryl benzimidazoles.

Effect of Ambient Pressure on the Axial Behavior of

Measurements of axial temperature and electron density have been carried out for Ar-H2 dc transferred arc-plasma columns under varying ambient-pressure conditions (100-760 torr). Optical emission spectroscopy has been used as the diagnostic tool. Temperature was determined by the relative intensity method using atomic hydrogen lines. The electron-density measurements were obtained from the Stark width of the Hß (486.13 nm) line. Possible deviation from local thermodynamic equilibrium (LTE) has been studied by using Hß transitions and by measuring the population factor using ArI (696.5 nm) transition. The nonideality along the plasma column has been studied using the electron-density data. The plasma approaches weakly nonideal conditions near substrate. The maximum deviation from LTE conditions also arises near the transferred anode substrate. With an increase in pressure, the volume of plasma approaches LTE.

\hbox{Ar}{-}\hbox{H}_{2}

The oxidation of aluminium was studied using optical emission spectroscopy (OES) during the evaporation of aluminium in traces of oxygen in a thermal plasma reactor. The ratio of the measured line intensities of Al-O with that of Al follows the exact trend as of that obtained from the corresponding line intensities in X-ray diffraction spectra of the synthesized samples. In this paper the inherent capacity of emission spectroscopy in evaluating the growth processes under plasma induced reactions is presented.

Transferred Thermal Arc-Plasma Column

This paper for the first time reports the (200) oriented growth of hexagonal Aluminum nitride crystals during synthesis of aluminum nanoparticles in dc transferred arc thermal plasma reactor by gas phase condensation in nitrogen plasma. The structural and morphological study of as synthesized AlN crystal and aluminium nanoparticles was done by using the x‐ray diffraction method, scanning electron microscopy and transmission electron microscopy.