We investigated the effect of temperature on the growth rate and structure of carbon nanotubes using scanning electron microscopy, transmission electron microscopy, and Raman spectroscopy. The carbon nanotubes were grown vertically aligned on iron nanoparticle deposited silicon substrate by thermal chemical vapor deposition of acetylene in the temperature range 800-1100 °C. As the growth temperature increases from 800 to 1100 °C, the average diameter increases from 20 to 150 nm and the growth rate also increases by about 20 times. All carbon nanotubes exhibit a bamboo-like structure over this temperature range. In the carbon nanotubes grown at higher temperature, the thicker compartment layers appear more frequently. The relative amount of crystalline graphitic sheets increases progressively with the growth temperature. The Arrhenius plot provides the activation energy of carbon nanotube growth to be at least 30 kcal/mol. The results indicate that the bulk diffusion of carbons would be an important factor in the growth of carbon nanotubes.
Wet-chemical etching of the barrier oxide layer of anodic aluminum oxide (AAO) was systematically investigated by using scanning electron microscopy (SEM), secondary ion mass spectrometry (SIMS), and a newly devised experimental setup that allows accurate in situ determination of the pore opening point during chemical etching of the barrier oxide layer. We found that opening of the barrier oxide layer by wet-chemical etching can be significantly influenced by anodization time (tanodi). According to secondary ion mass spectrometry (SIMS) analysis, porous anodic aluminum oxide (AAO) samples formed by long-term anodization contained a lower level of anionic impurity in the barrier oxide layer compared to the short-term anodized one and consequently exhibited retarded opening of the barrier oxide layer during the wet-chemical etching. The observed compositional dependence on the anodization time (tanodi) in the barrier oxide layer is attributed to the progressive decrease of the electrolyte concentration upon anodization. The etching rate of the outer pore wall at the bottom part is lower than that of the one at the top part due to the lower level of impurity content in that region. This indicates that a concentration gradient of anionic impurity in the outer pore wall oxide may be established along both the vertical and radial directions of cylindrical pores. Apart from the effect of electrolyte concentration on the chemical composition of the barrier oxide layer, significantly decreased current density arising from the lowered concentration of electrolyte during the long-term anodization (~120 h) was found to cause disordering of pores. The results of the present work are expected to provide viable information not only for practical applications of nanoporous AAO in nanotechnology but also for thorough understanding of the self-organized formation of oxide nanopores during anodization.
Atomically precise fabrication methods are critical for the development of next-generation technologies. For example, in nanoelectronics based on van der Waals heterostructures, where two-dimensional materials are stacked to form devices with nanometer thicknesses, a major challenge is patterning with atomic precision and individually addressing each molecular layer. Here we demonstrate an atomically thin graphene etch stop for patterning van der Waals heterostructures through the selective etch of two-dimensional materials with xenon difluoride gas. Graphene etch stops enable one-step patterning of sophisticated devices from heterostructures by accessing buried layers and forming one-dimensional contacts. Graphene transistors with fluorinated graphene contacts show a room temperature mobility of 40,000 cm2 V−1 s−1 at carrier density of 4 × 1012 cm−2 and contact resistivity of 80 Ω·μm. We demonstrate the versatility of graphene etch stops with three-dimensionally integrated nanoelectronics with multiple active layers and nanoelectromechanical devices with performance comparable to the state-of-the-art.
Nitrogen-doped carbon nanotubes were grown vertically aligned on the iron nanoparticles deposited on silicon substrates, by thermal chemical vapor deposition of methane/ammonia and acetylene/ammonia mixtures in the temperature range 900-1100 °C. The concentration of the nitrogen atoms has been controlled in the range 2-6 atomic %, by the flow rate of ammonia. All nanotubes exhibit a bamboo-like structure over this temperature range. The growth rate is insensitive to this nitrogen content, but the structure is strongly dependent on it. As the nitrogen content increases, the thicker compartment layers form uniformly at a regular distance and the relative amount of crystalline graphitic sheets is notably reduced. Electron energy-loss spectroscopy reveals the higher nitrogen concentration and the lower crystallinity for the compartment layers compared to the wall. The growth of nitrogen-doped carbon nanotubes has been explained using a base growth mechanism proposed for carbon nanotubes. We suggest that the nitrogen doping would produce more flexible compartment layers connecting the wall under a less strain.
A new compound material of 2D hydrofluorinated graphene (HFG) is demonstrated whose relative hydrogen/fluorine concentrations can be tailored between the extremes of either hydrogenated graphene (HG) and fluorinated graphene (FG). The material is fabricated through subsequent exposures to indirect hydrogen plasma and xenon difluoride (XeF2). Controlling the relative concentration in the HFG compound enables tailoring of material properties between the extremes offered by the constituent materials and in‐plane patterning produces micrometer‐scale regions with different surface properties. The utility of the technique to tailor the surface wettability, surface friction, and electrical conductivity is demonstrated. HFG compounds display wettability between the extremes of pure FG with contact angle of 95° ± 5° and pure HG with contact angle of 42° ± 2°. Similarly, the HFG surface friction may be tailored between the two extremes. Finally, the HFG electrical conductivity tunes through five orders of magnitude when transitioning from FG to HG. When combined with simulation, the electrical measurements reveal the mechanism producing the compound to be a dynamic process of adatom desorption and replacement. This study opens a new class of 2D compound materials and innovative chemical patterning with applications for atomically thin 2D circuits consisting of chemically/electrically modulated regions.
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