Investigations of carbon nanotubes

Experiments have been carried out to optimize the yields of carbon nanotubes obtained by the arc-evaporation of graphite. Other types of carbon particles such as nanocrystalline graphite usually present along with the nanotubes are readily removed by heating the material in oxygen around 763 K. Clean nanotubes so obtained have been characterized by X-ray diffraction. The clean tubes are thermally more stable than graphite or fullerenes. The tips of carbon nanotubes are opened by reaction with oxygen, but more interestingly, when the oxygen produced by the decomposition of a metal oxide is used to open the tube tips, the metal formed in the process enters the nanotube. Electrical resistance of pressed pellets of clean tubes is not unlike that of graphite. Tunnelling conductance measurements on isolated tubes characterized by means of scanning tunnelling microscopy however show that the conductance gap increases with decreasing tube diameter.

Orientational disorder and other aspects of C70 and C60-C70 films deposited on single-crystal substrates

C-70 films deposited on highly oriented pyrolytic graphite (HOPG), Ag(110), Ag(111) and Pt(110) substrates have been investigated by scanning tunnelling microscopy. Interesting observations on novel molecular arrangements, as well as orientational disorder, are presented. Solid solutions of C-60 and C-70 show interesting packing of these molecules when deposited on HOPG.

Metal-organic chemical vapour deposition of thin films of cobalt on different substrates: study of microstructure

We have investigated the microstructure of thin films grown by metal-organic chemical vapour deposition using a beta-diketonate complex of cobalt, namely cobalt (11) acetylacetonate. Films were deposited on three different substrates: Si(100), thermally oxidised silicon [SiO2/Si(100)] and glass at the same time. As-grown films were characterised by X-ray diffraction, scanning electron microscopy, scanning tunnelling microscopy, atomic force microscopy and secondary ion mass spectrometry. Electrical resistivity was measured for all the films as a function of temperature. We found that films have very fine grains, resulting in high electrical resistivity Further, film microstructure has a strong dependence on the nature of the substrate and there is diffusion of silicon and oxygen into cobalt from the substrate. (C) 2002 Elsevier Science B.V. All rights reserved.

Explosives Sensing by Using Electron-Rich Supramolecular Polymers: Role of Intermolecular Hydrogen Bonding in Significant Enhancement of Sensitivity

We demonstrate here that supramolecular interactions enhance the sensitivity towards detection of electron-deficient nitro-aromatic compounds (NACs) over discrete analogues. NACs are the most commonly used explosive ingredients and are common constituents of many unexploded landmines used during World WarII. In this study, we have synthesised a series of pyrene-based polycarboxylic acids along with their corresponding discrete esters. Due to the electron richness and the fluorescent behaviour of the pyrene moiety, all the compounds act as sensors for electron-deficient NACs through a fluorescence quenching mechanism. A Stern-Volmer quenching constant determination revealed that the carboxylic acids are more sensitive than the corresponding esters towards NACs in solution. The high sensitivity of the acids was attributed to supramolecular polymer formation through hydrogen bonding in the case of the acids, and the enhancement mechanism is based on an exciton energy migration upon excitation along the hydrogen-bond backbone. The presence of intermolecular hydrogen bonding in the acids in solution was established by solvent-dependent fluorescence studies and dynamic light scattering (DLS) experiments. In addition, the importance of intermolecular hydrogen bonds in solid-state sensing was further explored by scanning tunnelling microscopy (STM) experiments at the liquid-solid interface, in which structures of self-assembled monolayer of the acids and the corresponding esters were compared. The sensitivity tests revealed that these supramolecular sensors can even detect picric acid and trinitrotoluene in solution at levels as low as parts per trillion (ppt), which is much below the recommended permissible level of these constituents in drinking water.

A High-Resolution Transmission of the Precipitation Process in a Electron Microscopy Study Dilute Ti-N Alloy

The precipitation processes in dilute nitrogen alloys of titanium have been examined in detail by conventional transmission electron microscopy (CTEM) and high-resolution electron microscopy (HREM). The alloy Ti-2 at. pct N on quenching from its high-temperature beta phase field has been found to undergo early stages of decomposition. The supersaturated solid solution (alpha''-hcp) on decomposition gives rise to an intimately mixed, irresolvable product microstructure. The associated strong tweed contrast presents difficulties in understanding the characteristic features of the process. Therefore, HREM has been carried out with a view to getting a clear picture of the decomposition process. Studies on the quenched samples of the alloy suggest the formation of solute-rich zones of a few atom layers thick, randomly distributed throughout the matrix. On aging, these zones grow to a size beyond which the precipitate/matrix interfaces appear to become incoherent and the alpha' (tetragonal) product phase is seen distinctly. The structural details, the crystallography of the precipitation process, and the sequence of precipitation reaction in the system are illustrated.

Damage assessment of basaltic rock mass due to repeated blasting in a railway tunnelling project - A case study

The demand for tunnelling and underground space creation is rapidly growing due to the requirement of civil infrastructure projects and urbanisation. Blasting remains the most inexpensive method of underground excavations in hard rock. Unfortunately, there are no specific safety guidelines available for the blasted tunnels with regards to the threshold limits of vibrations caused by repeated blasting activity in the close proximity. This paper presents the results of a comprehensive study conducted to find out the effect of repeated blast loading on the damage experienced by jointed basaltic rock mass during tunnelling works. Conducting of multiple rounds of blasts for various civil excavations in a railway tunnel imparted repeated loading on rock mass of sidewall and roof of the tunnel. The blast induced damage was assessed by using vibration attenuation equations of charge weight scaling law and measured by borehole extensometers and borehole camera. Ground vibrations of each blasting round were also monitored by triaxial geophones installed near the borehole extensometers. The peak particle velocity (V-max) observations and plastic deformations from borehole extensometers were used to develop a site specific damage model. The study reveals that repeated dynamic loading imparted on the exposed tunnel from subsequent blasts, in the vicinity, resulted in rock mass damage at lesser vibration levels than the critical peak particle velocity (V-cr). It was found that, the repeated blast loading resulted in the near-field damage due to high frequency waves and far-field damage due to low frequency waves. The far field damage, after 45-50 occurrences of blast loading, was up to 55% of the near-field damage in basaltic rock mass. The findings of the study clearly indicate that the phenomena of repeated blasting with respect to number of cycles of loading should be taken into consideration for proper assessment of blast induced damage in underground excavations.

In situ transmission electron microscopy study of deformation of an aluminum alloy tribolayer

Nanoscale deformation in the tribolayer of an Al–Mg alloy is studied using an in situ mechanical probe in a transmission electron microscope. The sample is strained locally at room temperature and the deformation is observed in real time. It is observed that when the tungsten probe comes into contact with the tribolayer, the material exhibits further hardening followed by material removal.

Scanning electron microscopy study of worn Al-Si alloy surfaces

A pin-on-disc machine was used to wear Al-Si alloy pins under dry conditions. Unmodified and modified binary alloys and commercial multi-component alloys were tested. The surfaces of the worn alloys were examined by scanning electron microscopy to identify distinct topographical features to aid elucidation of the mechanisms of wear.

Structural origin of set-reset processes in Ge15Te83Si2 glass investigated using in situ Raman scattering and transmission electron microscopy

We report here that the structural origin of an easily reversible Ge15Te83Si2 glass can be a promising candidate for phase change random access memories. In situ Raman scattering studies on Ge15Te83Si2 sample, undertaken during the amorphous set and reset processes, indicate that the degree of disorder in the glass is reduced from off to set state. It is also found that the local structure of the sample under reset condition is similar to that in the amorphous off state. Electron microscopic studies on switched samples indicate the formation of nanometric sized particles of c-SiTe2 structure. ©2009 American Institute of Physics

High Resoulution Electron Microscopy of Chloritoid Minerals From Different Geological Melieu

Structural defects of three chloritoid minerals from distinet geologic melieu have been investigated by high resolution electron microscopy. X-ray powder and electron diffraction patterns indicate that the chloritoid from one geological source (A) is2M 1+2M2 monoclinic variant while those from another geological source (B) are 2M 2 monoclinic variants. In a typical one-dimensional lattice image of a crystal from sourceA, the 2M 2 matrix is broken by insertion of triclinic inter-growths. Another crystal with the 2M 2 matrix showed single, triple, quadruple and quintuple layers displaying an unusually high degree of disorder. Lattice images of 2M 2 monoclinic variants from sourceB yielded more homogeneous micrographs. The important finding from the present studies is that the chloritoid from sourceA is a severely disordered low-temperature intermediate phase in the conversion of the triclinic chloritoid to the high-temperature ordered monoclinic variants of sourceB. Severely disordered chloritoids, marking the beginning of low grade metamorphism, are generated as intermediates between the state of complete disordered arrangement towards the end of low grade metamorphism within the narrow stability range of 400°–500°C.

Scanning electron microscopy studies of wear in LM13 and LM13-graphite particulate composite

Examination of the structure of worn surfaces has shown that the wear of LM13 and LM13-graphite particulate composite is controlled by the nature and extent of subsurface deformation. The addition of graphite influences the wear characteristics by affecting the plastically deformed zone. The possible mechanisms of wear are discussed.

Nano-meter scale plasticity in KBr studied by nanoindenter and force microscopy

The early stages of plasticity in KBr single crystals have been studied by means of nano-meter-scale indentation in complementary experiments using both a nanoindenter and an atomic force microscope. Nanoindentafion experiments precisely correlate indentation depth and forces, while force microscopy provides high-resolution force measurements and images of the surface revealing dislocation activity. The two methods provide very similar results for the onset of plasticity in KBr. Upon loading we observe yield of the surface in atomic layer units which we attribute to the nucleation of single dislocations. Unloading is accompanied by plastic recovery as evident from a non-linear force distance unloading curve and delayed discrete plasticity events.

Combined Atomic Force Microscopy and Modeling Study of The Evolution of Octadecylamine Films on a Mica Surface

The time evolution of the film thickness and domain formation of octadecylamine molecules adsorbed oil a mica surface is investigated Using atomic force microscopy. The adsorbed Film thickness is determined by measuring the height profile across the mica-amine interface of a mica surface partially immersed in a 15 mM solution of octadecylamine in chloroform. Using this novel procedure, adsorption of amine on mica is found to occur in three distinct stages, with morphologically distinct domain Formation and growth occurring during each stage. In the first stage, where adsorption is primarily in the thin-film regime, all average Film thickness of 0.2 (+/- 0.3) nm is formed for exposure times below 30 s and 0.8 (+/- 0.2) nm for 60 s of immersion time. During this stage, large sample spanning domains are observed. The second stage, which occurs between 60-300 s, is associated with it regime of rapid film growth, and the film thickness increases from about 0.8 to 25 nm during this stage. Once the thick-film regime is established, further exposure to the amine solution results in all increase in the domain area, and it regime of lateral domain growth is observed. In this stage, the domain area coverage grows from 38 to 75%, and the FTIR spectra reveal an increased level of crystallinity in the film. Using it diffusion-controlled model and it two-step Langmuir isotherm, the time evolution of the film growth is quantitatively captured. The model predicts the time at which the thin to thick film transition occurs as well its the time required for complete film growth at longer times. The Ward-Tordai equation is also solved to determine the model parameters in the monolayer (thin-film) regime, which occurs during the initial stages of film growth.

Multiple excitation nano-spot generation and confocal detection for far-field microscopy

An imaging technique is developed for the controlled generation of multiple excitation nano-spots for far-field microscopy. The system point spread function (PSF) is obtained by interfering two counter-propagating extended depth-of-focus PSF (DoF-PSF), resulting in highly localized multiple excitation spots along the optical axis. The technique permits (1) simultaneous excitation of multiple planes in the specimen; (2) control of the number of spots by confocal detection; and (3) overcoming the point-by-point based excitation. Fluorescence detection from the excitation spots can be efficiently achieved by Z-scanning the detector/pinhole assembly. The technique complements most of the bioimaging techniques and may find potential application in high resolution fluorescence microscopy and nanoscale imaging.

Preparation, characterization and electrical conductivity studies of MWCNT/ZnO nanoparticles hybrid

Multiwall carbon nanotubes (MWCNTs) were decorated with crystalline zinc oxide nanoparticles (ZnO NPs) by wet chemical route to form MWCNT/ZnO NPs hybrid. The hybrid sample was characterized by scanning and transmission electron microscopy, X-ray diffraction and X-ray photoelectron spectroscopy. Electrical conductivity of the hybrid can be tuned by varying the ZnO NPs content in the hybrid. In order to investigate the effect of nanoparticles loading on the conduction of MWCNTs network, electrical conductivity studies have been carried out in the wide temperature range 1.5-300K. The electrical conductivity of the hybrid below 100K is explained with the combination of variable range hopping conduction and thermal fluctuation induced tunnelling model. (C) 2009 Elsevier B.V. All rights reserved.