Effect of processing temperature on growing bamboo-like carbon nanotubes by chemical vapor deposition

The present article demonstrates a simple, eco-friendly route for the fabrication of carbon nanotubes (CNTs) with different morphologies, including the fascinating bamboo-like structures without complex catalyst/support preparation procedures. A thermal chemical vapor deposition (CVD) technique that utilized natural pozzolan supports and a solid carbon source, that is, a mixture of camphor and ferrocene in a weight ratio of 20:1, was carried out at different temperatures where the ferrocene played also the role of catalyst. The pozzolan chemical composition and mineral identification were determined by energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy. The morphology of the fabricated CNTs was studied via scanning and transmission electron microscopies (SEM and TEM). It was revealed that both conventional tubular and bamboo-like nanotubes grow at 750 °C while the bamboo-like morphology prevails at 850 °C. The better nanostructure uniformity at higher deposition temperature was accompanied by an improved nanotube graphitization degree that was verified by Raman spectroscopy. Yet, the reduction of the CNTs production yield was recorded by thermogravimetric analysis (TGA). The experimental data are interpreted and discussed as an interplay between the CNTs processing temperature, morphology and growth mechanism. Thus, the growth of either tubular or bamboo-like nanostructures is suggested to be ruled by the competitive surface and bulk diffusions of carbon onto and into the catalyst surface. The growth depends on the size of catalyst nanoparticles sintered at different temperatures. The favorable role of the pozzolan supporting materials in the formation of bamboo-like tubes is emphasized.     

Synthesis of C–N nanotube blocks and Y-junctions in bamboo-like C–N nanotubes

We report the observations made on the synthesis and characterization of C–N nanotube blocks and Y-junctions in bamboo-like C–N nanotubes. The C–N nanotube Blocks have been synthesized by pyrolyzing the mixture of silver nitrate acetonitrile solution and ferrocene benzene solution. The structural/microstructural characterization of the as-synthesized material has been done using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). X-ray photoelectron spectroscopic (XPS) analysis has been carried out to confirm the presence of nitrogen in nanotubes. These investigations reveal the formation of blocks of bamboo-like nanotubes having the dimension 300 × 200 × 30 μm and the diameter is 20–50 nm. We also observe the formation of Y-junctions in bamboo-like nanotubes as we spray the acetonitrile ferrocene and AgNO₃ mixture. The length of the synthesized Y-junction nanotube bundles is ~2 μm. Some more complex Ψ-shaped junctions are also found to be present. The diameters of the Y-junction nanotubes is ~80 nm at the junction and 25–50 nm at the branches.     

Synthesis of Nitrogen Incorporated Carbon Nanotubes with Different Diameters by Catalytic Pyrolysis of Butylamine

Bamboo-like nitrogen-doped carbon(CNx) nanotubes were synthesized by chemical vapor deposition (CVD) at a high reaction temperature of 600―900 °C. The butylamine and Fe/SBA-15 molecular sieve have been used as precursor and catalyst, respectively. Transmission electron microscopy(TEM) and high resolution transmission electron microscopy(HRTEM) observations show that the outer diameter and wall thickness as well as the inner diameter were increased with increasing reaction temperature in a temperature range of 600―800 °C. A synergism mechanism of the growth through bulk diffusion and the competitive growth through surface diffusion functions during the synthesis of CNx nanotubes was proposed.     

Research on bamboo-like one dimensional o-BN nanowire

Orthorhombic boron nitride (oBN) nanowires with diameters ranging from 50–100 nm and lengths up to several tens micrometers was synthesized in a simple hydrothermal route. The as prepared sample has been characterized as oBN by SEM, HRTEM and SADP. Based on careful observation, unique bamboo-like nanostructures was found in the products. A probable formation mechanism of bamboo-like nanowires was discussed.     

Synthesis and characterization of nanocarbon having different morphological structures by chemical vapor deposition over Fe-Ni-Co-Mo/MgO catalyst

Catalytic chemical vapor deposition (CCVD) is one of the most promising synthesis methods for economically producing large quantities of different nanocarbon structures. Here we report a systematic study of the synthesis conditions for the preparation of different nanocarbon morphological structures via acetylene decomposition over the surface of quaternary-metallic catalyst (Fe-Ni-Co-Mo) supported on MgO (Fe-Ni-Co-Mo/MgO). In particular, the effect of temperature, and the reaction time were investigated to optimize the yield, quality, size and graphitic crystallinity of the deposited carbon. The study showed a successful synthesis of: (i) a high-yield and quality bamboo-like multiwalled carbon nanotubes (b-CNT), (ii) hybrid graphene/carbon nanotubes (G/CNT), and (iii) multilayer graphene (MLG). The structures of the obtained products were characterized by HR-TEM, TGA, Raman spectroscopy, FTIR and X-ray diffraction. The results found seem essential for realizing the role of different synthesis parameters on the yield, quality, and morphology of the synthesized product.     

竹节状α-Fe2O3纳米棒的制备、表征和性能研究

以硝酸铁为铁源,氨水为沉淀剂,聚乙二醇(PEG)为分散剂,采用共沉淀法制备氢氧化铁前驱体,然后将获得的前驱体在450℃、氮气保护下热处理2 h,最后利用透射电镜、X射线衍射、拉曼光谱和近边X射线精细结构光谱(NEXAFs)表征样品的形貌和结构,并使用HH-50型振动样品磁强计测量样品在室温下的磁学行为.透射电镜结果显示,获得的样品由氧化铁纳米颗粒和竹节状氧化铁纳米棒组成,纳米颗粒的粒径范围为50～100 nin,纳米棒的直径大约为10 nin.XRD表征显示样品中氧化铁纳米棒和纳米颗粒为赤铁矿型α-Fe2O3;光谱实验结果证实了样品中氧化铁纳米颗粒和纳米棒的结构是α-Fe2O3;磁学性能测试表明获得的样品表现为典型铁磁性材料的磁滞回线,其饱和磁感应强度约为64.65 emu·g-1,矫顽力的大小约为15.13 Oe.     

Catalytic synthesis of bamboo-like multiwall BN nanotubes via SHS-annealing process

Bamboo-like multiwall boron nitride (BN) nanotubes were synthesized via annealing porous precursor prepared by self-propagation high temperature synthesis (SHS) method. The as-synthesized BN nanotubes were characterized by the field emission scanning electron microscopy (FE-SEM), transmission electron microscope (TEM), high-resolution TEM (HRTEM), X-ray diffraction (XRD), Raman and Fourier transform infrared (FTIR) spectroscopy. These nanotubes have uniform diameters of about 60 nm and an average length of about 10 μm. Four growth models, including tip, base, based tip and base-tip growth models, are proposed based on the catalytic vapor-liquid-solid (VLS) growth mechanism for explaining the formation of the as-synthesized bamboo-like BN nanotubes. Chemical reactions and annealing mechanism are also discussed.