Observation of inversion domain boundaries in Mg-doped AlGaN layers grown by metalorganic chemical vapor deposition

We have investigated the formation of inversion domain boundaries in Al_0.13Ga_0.87N layers grown on sapphire substrates by metalorganic chemical vapor deposition using transmission electron microscopy (TEM). We found that the shape of inversion domain boundaries strongly depends on Mg source flow rate in the Mg-doped Al_0.13Ga_0.87N layers. By increasing the Mg source flow rate, the shape of inversion domain boundaries is changed from the vertical shape to the horizontal shape. In addition, the change of polarity by the horizontal shape inversion domain boundary (IDB) resulted in the inverted rotation of pyramidal shape IDB within the Mg-doped Al_0.13Ga_0.87N layers.     

Electrospun precursor carbon nanofibers optimization by using response surface methodology

Ultrafine fibers were electrospun from Polyacrylonitrile and N,N-dimethylformamide solution to be used as a precursor for carbon nanofibers. An electrospinning set-up was used to collect fibers with diameter ranging from 104 nm to 434 nm. Morphology of fibers and its distribution were investigated by varying Berry's number, charge density, spinning angle, spinneret diameter and collector area. A more systematic understanding of process parameters was obtained and a quantitative relationship between electrospinning parameters and average fiber diameter was established by using response surface methodology. It was concluded that; Berry's number, charge density and spinneret diameters played an important role to the diameter of nanofibers and its standard deviation. Spinning angle and collector area had no significant impact. Based on response surface methodology the optimum Polyacrylonitrile average fiber diameter of 280 nm and 28 nm standard deviation, were collected at 1.6 kV/cm charge density, 8 Berry's number and 0.9 mm spinneret diameter.     

Structural and morphological properties of thin ZnO films grown by pulsed laser deposition

The pulsed laser deposition technique was used to produce zinc oxide thin films onto silicon and Corning glass substrates. Homogeneous surfaces exhibiting quite small Root Mean Square (RMS) roughness, consisting of shaped grains were obtained, their grain diameters being 40-90 nm at room temperature and at 650 °C growth respectively. Films were polycrystalline, even for growth at room temperature, with preferential crystallite orientation the (0 0 2) basal plane of wurtzite ZnO. Temperature increase caused evolution from grain to grain agglomeration structures, improving crystallinity. Compressive to tensile stresses transition with temperature was found while the lattice constant decreased.     

Catalyst influence on the flame synthesis of aligned carbon nanotubes and nanofibers

Since prepared substrates offer an appropriate method for the selective production of uniform arrays of aligned CNTs and CNFs, it is important to illustrate the influence of different catalysts on the resulting nanostructures. This investigation characterizes the activity of three catalysts—iron in alloyed form as stainless steel, nickel, and platinum—on carbon nanostructure formation under identical conditions in an ethylene/air nonpremixed flame. We have synthesized well-aligned multi-walled CNTs (on Ni) and CNFs (on stainless steel). The third transition metal Pt produces CNF structures of a different kind, and its activity has not been previously characterized in flames. The catalyst and gas-phase conditions leading to the formation of these different structures are discussed.     

Carbon fractals grown from carbon nanotips by plasma-enhanced hot filament chemical vapor deposition

Carbon nanomaterials with different structures were prepared in a custom-designed plasma-enhanced hot filament chemical vapor deposition system using methane, hydrogen and nitrogen. They were investigated by scanning electron microscopy (SEM) and micro-Raman spectroscopy. The SEM images show that the smooth carbon nanotips are formed under a high bias current and the carbon fractals can grow from the tips of the carbon nanotips under a low bias current. The results of micro-Raman spectroscopy indicate that the graphitization of the carbon nanomaterials was improved by ion bombardment. Combined the ion bombardment, electric field enhancement and electron emission mechanisms, the formation model of the carbon fractals was suggested.     

Effect of sulfur on the growth of carbon nanotubes by detonation-assisted chemical vapor deposition

Thiophene was introduced as an additive in detonation-assisted chemical vapor deposition to investigate the effect of sulfur on the growth of carbon nanotubes. The results reveal that sulfur promoted the growth of hollow tubes, instead of bamboo-like carbon nanotubes without sulfur addition. Structural characterization of products indicates that the dynamic reshaping of the catalyst assisted bamboo-like carbon nanotube growth and the bamboo knots preferentially nucleated on the Ni-graphite step edges. It is suggested that sulfur suppressed the bamboo knot growth through blocking the step sites. The findings are important for understanding of nanotube growth mechanism and the role of sulfur often involved in catalytic reactions.     

Catalytic activity of Fe, Co and Fe-Co-MCM-41 for the growth of carbon nanotubes by chemical vapour deposition method

Iron, cobalt and a mixture of iron and cobalt incorporated mesoporous MCM-41 molecular sieves were synthesised by hydrothermal method and used to investigate the rules governing their nanotube producing activity. The catalysts were characterised by XRD and N₂ sorption studies. The effect of the catalysts has been investigated for the production of carbon nanotubes at an optimised temperature 750 °C with flow rate of N₂ and C₂H₂ is 140 and 60 ml/min, respectively for a reaction time 10 min. Fe-Co-MCM-41 catalyst was selective for carbon nanotubes with low amount of amorphous carbon with increase in single-walled carbon nanotubes (SWNTs) yield at 750 °C. Formation of nanotubes was studied using scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman spectroscopy. Transmission electron microscope and Raman spectrum was used to follow the quality and nature of carbon nanotubes formed and the graphitic layers and disordered band, which shows the clear evidence for the formation of SWNTs, respectively. The result propose that the diameter of the nanotubes in the range of 0.78-1.35 nm. Using our optimised conditions for this system, Fe-Co-MCM-41 showed the best results for selective SWNTs with high yield when compared with Fe-MCM-41 and Co-MCM-41.     

A detailed model for the flame synthesis of carbon nanotubes and nanofibers

Many experimental investigations of CNT/CNF flame synthesis have been recently reported. However, there are as yet no comprehensive models regarding their formation, growth or structure. Herein, a CNT/CNF growth rate model is proposed that is applicable for any method of CNT/CNF production (although our particular interest lies in flame synthesis in ethylene/air flames). While it is usual for most existing models to consider only a single carbon-carrying gas that contributes towards carbon deposition, our extended model can consider a complex hydrocarbon mixture that can mimic a flame environment. The model shows that before carbon nucleation is initiated, the surface density of carbon atoms increases as they are added through diffusion from the leading face of the catalyst nanoparticle. Over time, the diffusion potential decreases due to a reduction in the carbon atom concentration gradient. However, with the onset of nucleation and growth, diffusion is reinstated as the major driving potential for carbon atom transport through the nanoparticle. Steady carbon deposition and filament growth occurs once there is a stable carbon cluster size due to nucleation. The results support our hypothesis that flame synthesis can be a much faster and higher throughput process than CVD. The CNT/CNF growth rate decreases with increasing height above the burner. Decreasing temperature at higher locations leads to slower catalyst deactivation, but the CO concentration, which is the major contributor to carbon deposition, also decreases with increasing height above the burner. One of the major findings in this work is the contribution of CO to CNT formation by flame synthesis. The concentration of hydrocarbons in the vicinity of the toroidal zone near, which most of the CNT growth is observed, is negligible compared to CO concentration. Our results provide a basis to conduct future multiscale simulations of CNT/CNF growth.     

Synthesis and characterization of graphenated carbon nanotubes on IONPs using acetylene by chemical vapor deposition method

The graphenated carbon nanotubes (G-CNTs) were synthesized on monodisperse spherical iron oxide nanoparticles (IONPs) using acetylene as carbon precursor by simple chemical vapor deposition method. The reaction parameters such as temperature and flow of carbon source were optimized in order to achieve G-CNTs with excellent quality and quantity. Transmission electron microscopy (TEM) clearly illustrated that the graphene flakes are forming along the whole length on CNTs. The degree of graphitization was revealed by X-ray diffraction (XRD) analysis and Raman spectroscopic techniques. The intensity of D to G value was less than one which confirms the obtained G-CNTs have high degree of graphitization. The optimum reaction temperature for the IONPs to form metallic clusters which in turn lead to the formation of G-CNTs with high carbon deposition yield is at 900 °C. The TEM shows the CNTs diameter is 50 nm with foiled graphene flakes of diameter around 70 nm. Our results advocate for IONPs as a promising catalytic template for quantitative and qualitative productivity of nanohybrid G-CNTs. The produced G-CNTs with high degree of graphitization might be an ideal candidate for nanoelectronic application like super capacitors and so on.     

Analysis of HRTEM images for carbon nanostructure quantification

Image processing algorithms have been developed to extract fringe length, tortuosity and separation from high resolution transmission electron microscopy images. To validate the separation algorithm, a comparison is made between the image-based fringe separation and that obtained by analysis of X-ray diffraction data for a progressively heat-treated carbon black. Agreement is favorable. To illustrate the utility of the analysis parameters for a range of carbon nanostructures, analysis is applied to a series of pyrolytically prepared carbon soots – qualitatively described as containing amorphous, graphitic or fullerenic nanostructure. For all processing, the intermediate image, in the form of a skeletonized binary image of the original high resolution transmission electron micrograph, is shown and found to accurately reflect the nanostructural organization within the carbon as visually observed. Statistical results for each analysis parameter, extracted from the binary images, are presented in the form of histograms and quantitatively distinguish the different carbon nanostructures.     

XRD, HRTEM, magnetic and Mössbauer studies on chemically prepared Fe-doped nanoparticles of cerium oxide

Nanocrystalline samples of Fe-doped cerium oxide (Ce_0.90Fe_0.1O₂) are prepared by sol-gel method. The precursor materials used for the synthesis are ferric nitrate and cerium nitrate. The as-prepared samples is annealed at different temperatures to obtain the sample with different particle sizes. The crystallographic phases of the nanocrystalline materials have been confirmed by X-ray diffractograms (XRD). The sizes of the nanoparticles estimated from the peaks of the XRD patterns using Debye-Scherrer equation are in the range 6-58 nm. Results extracted from the high-resolution transmission electron microscopy (HRTEM) are in agreement with the findings obtained from XRD. The average magnetic susceptibilities of all the samples with different particle sizes are measured in the temperature range 300-14 K. The average susceptibilities of the samples annealed below ∼740 °C show paramagnetic behaviour. The susceptibilities of the samples annealed at and above ∼740 °C sharply decrease at ∼240 K and this sharp transition is quite likely due to the anti-parallel alignment of Fe³⁺ spins and is attributed to Morin transition of α-Fe₂O₃. Mössbauer spectra of the samples annealed at and above ∼740 °C give sextet patterns indicating the presence of exchange interaction among the Fe³⁺ ions of these samples and these sextets are also of typical nature of the α-Fe₂O₃ phase. The Mössbauer spectra of the samples annealed below ∼740 °C are doublets which may be attributed to either superparamagnetic and/or paramagnetic type nanoparticles.     

Hydrogen-induced buckling of Pd films studied by positron annihilation

Hydrogen loading of thin films introduces very high compressive stresses which grow in magnitude with increasing hydrogen concentration. When the hydrogen-induced stresses exceed a certain critical in-plane stress value, the loaded film starts to detach from the substrate. This results in the formation of buckles of various morphologies in the film layer. Defect studies of a hydrogen loaded Pd film which undergoes a buckling process are presented, using slow positron implantation spectroscopy, in situ acoustic emission, and direct observations of the film structure by transmission electron and optical microscopies. It is found that buckling of the film occurs at hydrogen concentrations x_H ≥ 0.1 and causes a significant increase of the dislocation density in the film.     

TEM study of annealed Pt nanostructures grown by electron beam-induced deposition

In this paper we report on the microstructural characterization of Pt nanostructures fabricated by electron beam-induced deposition in a dual beam system and subsequently annealed in furnace. The as-deposited nanostructures are made of a mixture of nanocrystalline Pt and amorphous carbon. We show by transmission electron microscopy and electron energy loss spectroscopy that the annealing in presence of oxygen at 550 °C for 30 min is able to remove the amorphous carbon from the nanostructure, leaving polycrystalline Pt grains.     

Photoemission investigations on nanostructured TiO2 grown by cluster assembling

Nanostructured titanium dioxide (ns-TiO₂) films were grown by supersonic cluster beam deposition method. Transmission electron microscopy demonstrated that films are mainly composed by TiO₂ nanocrystals embedded in an amorphous TiO₂ phase while their electronic structure was studied by photoemission spectroscopy. The cluster assembled ns-TiO₂ films are expected to exhibit several structural and chemical defects owing to the large surface to volume ratio of the deposited clusters. Ultraviolet photoemission spectra (hv = 50 eV) from the valence band unveil the presence of a restrained amount of surface Ti 3d defect states in the band gap, whereas Ti 2p core level X-ray photoelectron (hv = 630 eV) spectra do not manifestly disclose these defects.     

Structural properties of 10 μm thick InN grown on sapphire (0001)

The structural properties of a 10 μm thick In-face InN film, grown on Al₂O₃ (0001) by radio-frequency plasma-assisted molecular beam epitaxy, were investigated by transmission electron microscopy and high resolution x-ray diffraction. Electron microscopy revealed the presence of threading dislocations of edge, screw and mixed type, and the absence of planar defects. The dislocation density near the InN/sapphire interface was 1.55×10¹⁰ cm⁻², 4.82×10⁸ cm⁻² and 1.69×10⁹ cm⁻² for the edge, screw and mixed dislocation types, respectively. Towards the free surface of InN, the density of edge and mixed type dislocations decreased to 4.35×10⁹ cm⁻² and 1.20×10⁹ cm⁻², respectively, while the density of screw dislocations remained constant. Using x-ray diffraction, dislocations with screw component were found to be 1.2×10⁹ cm⁻², in good agreement with the electron microscopy results. Comparing electron microscopy results with x-ray diffraction ones, it is suggested that pure edge dislocations are neither completely randomly distributed nor completely piled up in grain boundaries within the InN film.     

Field emission characteristics of carbon nanotubes post-treated with high-density Ar plasma

The field emission characteristics of carbon nanotubes (CNTs) grown by thermal chemical vapor deposition (CVD) and subsequently surface treated by high-density Ar plasma in an inductively coupled plasma reactive ion etching (ICP-RIE) with the various plasma powers were measured. Results indicate that, after treated by Ar plasma with power between 250 and 500 W, the emission current density of the CNTs is enhanced by nearly two orders of magnitude (increased from 0.65 to 48 mA/cm²) as compared to that of the as-grown ones. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were employed to investigate the structural features relevant to the modified field emission properties of CNTs. The SEM images of CNTs subjected to a 500 W Ar plasma treatment exhibit obvious damages to the CNTs. Nevertheless, the turn-on fields decreased from 3.6 to 2.2 V/μm, indicating a remarkable field emission enhancement. Our results further suggest that the primary effect of Ar plasma treatment might be to modify the geometrical structures of the local emission region in CNTs. In any case, the Ar plasma treatment appears to be an efficient method to enhance the site density for electron emission and, hence markedly improving the electric characteristics of the CNTs.     

Improvement in performance of organic light-emitting devices by inclusion of multi-wall carbon nanotubes

Poly(3,4-ethylene dioxythiophene):poly(styrene sulfonate) (PEDOT:PSS) was modified by different concentrations of multi-wall carbon nanotubes (MWNTs), and the nanocomposites of PEDOT:PSS and MWNTs were firstly used as hole-injection layer in fabrication of organic light-emitting devices (OLEDs) by using a double-layer structure with hole-injection layer of doped PEDOT:PSS and emitting/electron transport layer of tris(8-hydroxyquinolinato) aluminum (Alq₃). PEDOT:PSS solution doped with MWNTs was spin-coated on clean polyethylene terephthalate (PET) substrate with indium tin oxide (ITO). It was found that the electroluminescence (EL) intensity of the OLEDs were greatly improved by using PEDOT:PSS doped with MWNTs as hole-injection layer which might have resulted from the hole-injection ability improvement of the nanocomposites. Higher luminescence intensity and lower turn-on voltage were obtained by these devices and the luminance intensity obtained from the device with the hole-injection layer of PEDOT:PSS doped by 0.4 wt.% MWNTs was almost threefolds of that without doping.     

Structural characterization of Ga-doped Mg0.1Zn0.9O layers grown on ZnO/α-Al2O3 templates by P-MBE

In this study, structural properties of epitaxial Ga-doped Mg_0.1Zn_0.9O layers grown on ZnO/α-Al₂O₃ templates by plasma-assisted molecular beam epitaxy have been investigated by high-resolution transmission electron microscopy (HRTEM), and high resolution X-ray diffraction (HRXRD). From analysis of the diffraction pattern, the monocrystallinity of the Mg_0.1Zn_0.9O layer with hexagonal structure is confirmed. The orientation relationship between Mg_0.1Zn_0.9O and the template is determined as (0 0 0 1)_Mg0.1Zn0.9O(0 0 0 1)_ZnO(0 0 0 1)_Al2O3 and [ [ ]_ZnO[ . The density of dislocations near the top surface layers measured by plan-view TEM is about 3.610¹⁰ cm⁻², one order of magnitude higher than the value obtained for ZnO layers on α-Al₂O₃ with a MgO buffer. Cross-sectional observation revealed that the majority of threading dislocations are in the [0 0 0 1] line direction, i.e. they lie along the surface normal and consist of edge, screw, and mixed dislocations. Cross- sectional TEM and X-ray rocking curve experiments reveal that most of dislocations are edge dislocations. The interface of Mg_0.1Zn_0.9O and ZnO layers and the effect of excess Ga-doping in these layers have been also studied.