Zoltán Osváth

Anomalies in thickness measurements of graphene and few layer graphite crystals by tapping mode atomic force microscopy

Atomic Force Microscopy (AFM) in the tapping (intermittent contact) mode is a commonly used tool to measure the thickness of graphene and few layer graphene (FLG) flakes on silicon oxide surfaces. It is a convenient tool to quickly determine the thickness of individual FLG films. However, reports from literature show a large variation of the measured thickness of graphene layers. This paper is focused on the imaging mechanism of tapping mode AFM (TAFM) when measuring graphene and FLG thickness, and we show that at certain measurement parameters significant deviations can be introduced in the measured thickness of FLG flakes. An increase of as much as 1 nm can be observed in the measured height of FLG crystallites, when using an improperly chosen range of free amplitude values of the tapping cantilever. We present comparative Raman spectroscopy and TAFM measurements on selected single and multilayer graphene films, based on which we suggest ways to correctly measure graphene and FLG thickness using TAFM.

Large scale production of short functionalized carbon nanotubes

A simple mechano-chemical modification of multiwall carbon nanotubes is described. The use of ball-milling in specific atmosphere allows us to introduce functional groups like thiol, amine, amide, carbonyl, chlorine, etc. onto carbon nanotubes. The resulted functional groups are characterized using infrared spectroscopy and X-ray photoelectron spectroscopy.

Synthesis and characterization of new polyaniline/nanotube composites

Abstract New polyaniline/nanotube (PANI/NT) composites have been synthesized by “in situ” polymerization processes using both multi-wall carbon nanotubes (MWNTs) and single-wall carbon nanotubes (SWNTs) in concentrations ranging from 2 to 50 wt.%. Although no structural changes are observed using MWNTs above a concentration of 20 wt.%, the in situ synthesis results in electronic interactions between nanotubes and the quinoid ring of PANI leading to enhanced electronic properties and thus to the formation of a genuine PANI/MWNT composite material. On the other hand, using SWNTs favors the formation of inhomogeneous mixtures rather than of a homogeneous composite materials, independent of the SWNT concentration. X-ray diffraction, Raman and transport measurements show the different behavior of both classes of nanotubes in PANI/NT materials. The difficulties in the formation of a true PANI/SWNT composite are related to the far more complex structure of the SWNT material itself, i.e. to the presence of entangled bundles of SWNTs, amorphous carbon and even catalytic metal particles.

Catalyst traces and other impurities in chemically purified carbon nanotubes grown by CVD

Multiwall carbon nanotubes grown by the catalytic decomposition of acetylene over supported Co catalyst were subjected to wet and dry oxidation in order to remove the unwanted products and the catalyst traces. The effects of the purification treatment on the Co content Ž. Ž . was monitored by physical methods: Rutherford Backscattering Spectrometry RBS , Particle Induced X-Ray Emission PIXE and Ž. X-Ray Fluorescence XRF . The purified products were investigated by microscopic methods: TEM, Scanning Electron Microscopy Ž. Ž . SEM , Energy Dispersive Spectroscopy EDS and STM. The KMnOrH SO aqueous oxidation procedure was found to be effective in 42 4 reducing the Co content while damaging only moderately the outer wall of the nanotubes. Treatment in HNO rH SO yields a 32 4 bucky-paper like product and produces the increase of the Si and S content of the sample. q 2002 Elsevier Science B.V. All rights reserved.

Room temperature growth of single-wall coiled carbon nanotubes and Y-branches

Abstract Straight carbon nanotubes, carbon nanotube “knees,” Y-branches of carbon nanotubes and coiled carbon nanotubes were grown on a graphite substrate held at room temperature by the decomposition of fullerene under moderate heating (450 °C) in the presence of 200-nm Ni particles. The grown structures were investigated without any further manipulation by STM. The growth and the chemical stability of the carbon nanostructures containing nonhexagonal rings are discussed.

Arc-grown Y-branched carbon nanotubes observed by scanning tunneling microscopy (STM)

Scanning tunneling microscopy (STM) observation of Y-branched carbon nanotubes produced by the arc-discharge method is reported. A drilled out graphite rod filled with a nickel/yttrium particle mixture was used as anode in the arc chamber under He atmosphere of 660-mbar pressure. Straight multi-wall nanotubes and asymmetrical Y-branches were found in a sample taken from the cathodic deposit. As measured by STM the Y-junctions have low apparent heights in the range of 1 nm. This may be an indication that these nanotubes have only few walls, or possibly they are single-walled. The asymmetrical Y-branches found in this experiment may be related to the additional use of metals or/and to changed temperature conditions on the cathode side due to the switch-off of the cathode water-cooling.

STM observation of asymmetrical Y-branched carbon nanotubes and nano-knees produced by the arc discharge method

The scanning tunneling microscopy (STM) observation of arc-grown Y-branched carbon nanotubes and sharp nanotube bends (nano-knees) is reported. A drilled out graphite rod filled with a nickel/yttrium particle mixture was used as the anode in an arc chamber under He atmosphere of 660-mbar pressure. Straight multi-wall nanotubes, Y-branches and nano-knees were found in a sample taken from the cathodic deposit. The asymmetrical Y-branches and complex nano-knees found in this experiment may be related to the additional use of metals or/and to induced changes of the temperature distribution on the cathode side. It is suggested that complex nano-knees could be new examples for carbon quantum dots.

STM and AFM investigation of coiled carbon nanotubes produced by laser evaporation of fullerene

Abstract Carbon nanotubes were grown by the evaporation of a fullerene/Ni particle mixture in vacuum, using 532 nm laser pulses of 12–28 μJ from a Nd YAG laser. The evaporated material was deposited on a freshly cleaved graphite (HOPG) surface and the samples were investigated by scanning tunneling microscopy (STM) and AFM. In the present work, we focus on the Y-branched and coiled carbon nanotubes, the formation of which supposes the incorporation of non-hexagonal rings in the hexagonal graphitic network. The regularity of the observed coils is an indication that the incorporation of the pentagons and heptagons occurred in a very regular way. The possible atomic structure of the coiled carbon nanotubes is discussed.

Controlling the nanoscale rippling of graphene with SiO2 nanoparticles

The electronic properties of graphene can be significantly influenced by mechanical strain. One practical approach to induce strain in graphene is to transfer atomically thin membranes onto pre-patterned substrates with specific corrugations. The possibility of using nanoparticles to impart extrinsic rippling to graphene has not been fully explored yet. Here we study the structure and elastic properties of graphene grown by chemical vapour deposition and transferred onto a continuous layer of SiO2 nanoparticles with diameters of around 25 nm, prepared on a Si substrate by the Langmuir-Blodgett technique. We show that the corrugation of the transferred graphene, and thus the membrane strain, can be modified by annealing at moderate temperatures. The membrane parts bridging the nanoparticles are suspended and can be reversibly lifted by the attractive forces between an atomic force microscope tip and graphene. This allows the dynamic control of the local morphology of graphene nanomembranes.

Ion beam mixing by focused ion beam

Si amorphous (41 nm)/Cr polycrystalline (46 nm) multilayer structure was irradiated by 30 keV Ga+ ions with fluences in the range of 25−820 ions∕nm2 using a focused ion beam. The effect of irradiation on the concentration distribution was studied by Auger electron spectroscopy depth profiling, cross-sectional transmission electron microscopy, and atomic force microscopy. The ion irradiation did not result in roughening on the free surface. On the other hand, the Ga+ irradiation produced a strongly mixed region around the first Si/Cr interface. The thickness of mixed region depends on the Ga+ fluence and it is joined to the pure Cr matrix with an unusual sharp interface. With increasing fluence the width of the mixed region increases but the interface between the mixed layer and pure Cr remains sharp. TRIDYN simulation failed to reproduce this behavior. Assuming that the Ga+ irradiation induces asymmetric mixing, that is during the mixing process the Cr can enter the Si layer, but the Si cannot enter the C...