Synthesis of NiO nanowalls by thermal treatment of Ni film deposited onto a stainless steel substrate

Two-dimensional nanostructures have a variety of applications due to their large surface areas. In this study, the authors present a simple and convenient method to realize two-dimensional NiO nanowalls by thermal treatment of a Ni thin film deposited by sputtering onto a stainless steel substrate. The substrate surface area is supposed to be significantly increased by creating nanowalls. The effects on the nanowall morphology of the thermal treatment temperature and duration are investigated. A mechanism based on the surface diffusion of Ni(2+) ions from the Ni?base film is then proposed for the growth of the NiO nanowalls. The as-synthesized NiO nanowalls are characterized by scanning electron microscopy, energy-dispersive x-ray analysis, x-ray diffraction, transmission electron microscopy and high resolution transmission electron microscopy.     

Controllable electrodeposition of ordered carbon nanowalls on Cu(111) substrates

We report the growth of amorphous carbon nanowalls with molten salt electrolytes and a carbonate carbon source at 600 °C on home-made Cu(111) foil as the growth substrate (and cathode). The nanometer thick nanowalls grow preferentially along symmetric slip lines on the Cu(111) surface and their ordered arrangement appears to also be dictated by the electrosynthesis parameters. Computational chemistry suggests that nucleation of carbon growth is favored at the slip lines (atomic steps) of the Cu(111) surface. The electrodeposited carbon structures can be varied by tuning the potential on the electrodes and temperature of the molten salt. The macro, micro, and nanoscale structure of the nanowalls was studied and is reported.     

Bias-independent growth of carbon nanowalls by microwave electron-cyclotron resonance plasma CVD

The investigations reported here describe the synthesis of carbon nanowalls (CNWs) by microwave electron-cyclotron resonance (ECR) plasma-assisted chemical vapour deposition (PACVD) process without an application of external bias to the substrate during growth. CNWs were grown on silicon (Si) substrates using hydrogen (H₂)/methane (CH₄) plasma at 650°C substrate temperature. Nickel (Ni) was used as a catalyst for the synthesis of CNWs. To the best of our knowledge, this is the first report that describes the bias-independent growth of CNWs using the ECR PACVD process. Formation of CNWs is confirmed by scanning electron microscopy and Raman spectroscopy. The discussion part also includes a possible growth mechanism for CNWs in terms of the role of surface plasmons.     

Solution growth of Cu2S nanowalls on Cu substrates and their characterization

A simple method of preparing Cu₂S nanowalls was presented by immersing Cu substrates into a Na₂S/HCl solution. X-ray diffraction (XRD) analysis revealed the formation of the monoclinic phase of Cu₂S nanostructures on Cu substrates, presenting a thickness of less than 100 nm and a height of several micrometers (called nanowalls) from the scanning electron microscopic (SEM) images. Moreover, the transmission electron microscopy (TEM) and X-ray energy dispersive spectrometry (EDS) characterizations indicated that these Cu₂S nanowalls were thinner near the sheet edge and had voids inside the sheets supposedly due to the etching reaction by Na₂S/HCl. Cu substrates with Cu₂S nanowalls were found to exhibit extinguished hydrophobicity (> 110°) resulting from their rough surfaces based on the water contact angle measurements. Electrical current-voltage analysis indicated the formation of a Schottky barrier at the Cu₂S/Cu interface.     

Hierarchical carbon nanostructure design: ultra-long carbon nanofibers decorated with carbon nanotubes

Hierarchical carbon nanostructures based on ultra-long carbon nanofibers (CNF) decorated with carbon nanotubes (CNT) have been prepared using plasma processes. The nickel/carbon composite nanofibers, used as a support for the growth of CNT, were deposited on nanopatterned silicon substrate by a hybrid plasma process, combining magnetron sputtering and plasma-enhanced chemical vapor deposition (PECVD). Transmission electron microscopy revealed the presence of spherical nanoparticles randomly dispersed within the carbon nanofibers. The nickel nanoparticles have been used as a catalyst to initiate the growth of CNT by PECVD at 600°C. After the growth of CNT onto the ultra-long CNF, SEM imaging revealed the formation of hierarchical carbon nanostructures which consist of CNF sheathed with CNTs. Furthermore, we demonstrate that reducing the growth temperature of CNT to less than 500°C leads to the formation of carbon nanowalls on the CNF instead of CNT. This simple fabrication method allows an easy preparation of hierarchical carbon nanostructures over a large surface area, as well as a simple manipulation of such material in order to integrate it into nanodevices.     

The effect of substrate morphology on the diameter distribution of carbon nanotubes grown on silica and ceramic substrates

Large-scale well-aligned carbon nanotube film and carbon nanotube bundles have been fabricated on smooth silica and rough polycrystalline ceramic substrates by pyrolysis of ferrocene/melamine mixtures. The images of transmission electron microscopy (TEM) and scanning electron microscope (SEM) show that carbon nanotubes grown on the silica substrate have uniform outer diameters of about ∼ 25 nm and lengths of about 40 μm, while those on the ceramic substrate have outer diameters from 10 to 90 nm and lengths up to 100 μm. Electron energy-loss spectroscopy (EELS) spectra show that nanotubes grown on the two different substrates are pure carbon tubes. The effects of substrate micro-morphologies on the diameters of carbon nanotubes have been discussed.     

A novel method for preparation of hollow and solid carbon spheres

Hollow and solid carbon spheres were prepared by the reaction of ferrocene and ammonium carbonate in a sealed quartz tube at 500°C. The morphology and microstructure of the product were characterized by X-ray diffraction, Raman spectroscopy, scanning electron microscopy and transmission electron microscopy. The carbon spheres are amorphous and their diameters range from 0·8–2·8 μm. The shell thickness of the hollow carbon spheres is not uniform and ranges from 100–180 nm. It is suggested that ammonium carbonate is crucial for the formation of carbon spheres and its amount also influences the morphology of the product. The method may be suitable for large scale preparation of carbon spheres.     

Copper nanowall array grown on bulk Fe-Co-Ni alloy substrate at room temperature as lithium-ion battery current collector

Large-scale copper nanowall array on the bulk Fe-Co-Ni alloy substrate has been prepared in aqueous solution at room temperature via an electroless deposition method. The thickness of the nanowalls is about 15 nm. A possible growth mechanism of the nanowalls was proposed. The effects of reaction temperature, reaction time and the amount of critical agent (Fe³⁺) on the morphology and crystalline phase of the nanowalls were investigated. Furthermore, the electrochemical performance of Sn film supported on the as-prepared copper nanowalls current collector is enhanced in comparison with that on the commercial copper foil when used as anode for Li-ion batteries with the operating voltage window of 0.01-2.0 V (vs. Li). After 20 cycles, the discharge capacity of Sn-Cu nanowalls anode still remained 365.9 mAh g^− 1, that is, 40% retention of the reversible capacity, while the initial charge capacity of Sn film cast on commercial Cu foil was 590 mAh g^− 1, dropping rapidly to 260 mAh g^− 1 only after 10 cycles.     

Synthesis and characterization of ZnO-In2O3 junction structure

Rod-shaped ZnO-In₂O₃ junction structure was obtained by bottom up approach of nanostructure fabrication and characterization. In₂Zn₃ alloy was evaporated in a tube furnace of 1150 °C temperature and 5 × 10⁻¹ Torr vacuum. The deposit collected on silicon wafer placed down stream of the tube furnace was examined by scanning electron microscope (SEM), energy dispersive x-ray spectroscopy (EDS), and transmission electron microscopy (TEM). SEM and EDS results proved the existence of rod-shaped ZnO-In₂O₃ junction structure. TEM analysis revealed the orientation relationship between ZnO and In₂O₃. It is suggested that this structure is formed via vapor-liquid-solid process and the suitable combination of source temperature, tube vacuum, and substrate temperature is the key for the formation of such novel structure. This report demonstrates the possibility of fabricating junction structure by bottom up approach, expanding its capability of fabricating structure with desired properties.     

In situ fabrication of carbon nanotube–MgAl2O4 nanocomposite powders through hydrogen-free CCVD

Carbon nanotube–MgAl₂O₄ composite powders were successfully prepared through solution combustion synthesis (SCS) followed by catalytic chemical vapor deposition (CCVD) of methane. Catalyst powders were synthesized starting with the stoichiometric ratios of metal nitrates and urea with a small amount of water and different Fe contents followed by subjecting the solution to heat. The obtained powders were placed in a silica tube to react with methane and form carbon nanotubes. It is noteworthy that no hydrogen was used throughout the whole process. Catalysts and composite powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman spectroscopy. The quality of products were evaluated by I_D/I_G ratio obtained from G and D bands intensities in Raman spectra of samples having 10 and 15 wt.% iron. The final product mostly comprised a mixture of single- and double-walled nanotubes on the catalyst containing 10 wt.% Fe, while no carbon product was formed on the catalyst with 5 wt.% Fe.     

Effect of substrate and catalyst on the transformation of carbon black into nanotubes

Structural transformation of carbon black (CB) into nanotubes and nano-onion like structures in the presence of bimetallic catalysts (Fe and Ni) is reported and the influence of the substrate (alumina and stainless steel) in the structural transformation is studied. In addition, the importance of a specific weight ratio of CB to catalyst in the transformation of amorphous CB into graphitic nanostructures is verified. The experiments were carried out at 1,000 °C in a horizontal tube furnace under N₂ atmosphere. The samples were characterized by transmission electron microscopy, high-resolution transmission electron microscopy, X-ray diffraction, Raman spectroscopy and also thermomagnetic analysis (Curie-temperature determinations) were done to assess thermally induced magnetic phase changes. All the characterization techniques showed the resulting structures were influenced by the substrate and weight ratio for CB to catalysts. However, there was no significant difference in the magnetic performance of the resulting structures obtained on different substrates.     

Cold-wall CVD carbon nanotube synthesis on porous alumina substrates

Carbon nanotubes were synthesized by chemical vapor deposition (CVD) using ethanol vapor as carbon source. Catalysts were Co and Mo metallic particles obtained from the corresponding acetates dissolved in ethanol. Acetate solutions are deposited on porous alumina substrates by dip coating. A dense array of aligned carbon nanotubes perpendicular to the substrate surface grow with 20 min exposure to ethanol vapor flow for substrate temperatures between 650 and 830 °C. Sample analysis is performed with scanning electron microscopy and Raman spectroscopy.     

Growth of carbon nanofibers and related structures by combined method of plasma enhanced chemical vapor deposition and aerosol synthesis

Growth of carbon nanofibers and nanotubes by combination of aerosol synthesis and plasma-enhanced catalytic chemical vapor deposition with alcohol as carbon precursor is presented. Only a hollow cathode glow discharge (HCGD) is used as gas activation process without any specific heating of the substrate. Specially designed hollow cathode enables the evaporation of catalyst directly on the substrate for catalytic growth. Product of physical vapor deposition process was examined by energy dispersive X-ray spectrometer (EDS). Spectroscopic features of the plasma were monitored by optical emission spectroscopy (OES). Carbon deposition was examined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Catalytic nanofibers and multi-walled carbon nanotubes with outer diameters 20-60 nm have been observed.     

Microstructures of GaN thin films grown on graphene layers

Plan-view and cross-sectional transmission electron microscopy images show the microstructural properties of GaN thin films grown on graphene layers, including dislocation types and density, crystalline orientation and grain boundaries. The roles of ZnO nanowalls and GaN intermediate layers in the heteroepitaxial growth of GaN on graphene, revealed by cross-sectional transmission electron microscopy, are also discussed.     

Carbon helixes produced by hot filament assisted chemical vapor deposition

Carbon helix nanofibers were synthesized by a hot filament assisted chemical vapor deposition at a substrate temperature of 600 °C. It was observed that the formation of a carbon helix structure was attributed to the mixing of cobalt catalyst particles with copper. The diameter of carbon helixes varied from 20 to 500 nm. The growth mechanism and the structure of these carbon helix nanofibers are discussed based on scanning electron microscopy and Raman spectroscopy measurements.     

Hot-wire chemical vapor deposition of carbon nanotubes

Hot-wire chemical vapor deposition (HWCVD) has been employed for the continuous gas-phase generation of both carbon multi-wall and single-wall nanotube (MWNT and SWNT) materials. Graphitic MWNTs were produced at a very high density at a synthesis temperature of 600 °C. SWNTs were deposited at a much lower density on a glass substrate held at 450 °C. SWNTs are typically observed in large bundles that are stabilized by tube–tube van der Waals’ interactions. However, transmission electron microscopy analyses revealed only the presence of isolated SWNTs in these HWCVD-generated materials.     

Controllable Synthesis of 3D Ni(OH)2 and NiO Nanowalls on Various Substrates for High‐Performance Nanosensors

Large‐area and uniform three‐dimensional (3D) β‐Ni(OH)₂ and NiO nanowalls were synthesized on a variety of rigid and flexible substrates via a simple aqueous chemical deposition process. The β‐Ni(OH)₂ nanowalls consist of single‐crystal Ni(OH)₂ nanosheets that were vertically grown on different substrates. The height, crystallinity, and morphology of the Ni(OH)₂ nanowalls can be readily modified by adjusting the reaction time and concentration of the NiCl₂ solution. The synthesis mechanism of the Ni(OH)₂ nanowalls was determined through heterogeneous nucleation and subsequent oriented crystal growth. 3D NiO nanowalls were obtained by thermal decomposition of the Ni(OH)₂ nanowalls at 400 °C in Ar atmosphere. Highly sensitive, selective gas sensors and electrochemical sensors based on these NiO nanowalls were developed. The chemiresistive gas sensors based on the NiO nanowalls grown on ceramic substrates exhibited an excellent performance with low detection limit for formaldehyde (8 ppb) and NO₂ (15 ppb). The electrochemical sensor based on the NiO nanowalls grown on an FTO glass substrate had a superior selectivity to non‐enzymatic glucose with a detection limit of 200 nm .     

Growth of mane-like ZnS nanostructures by using a two-heating zone-tube furnace: structural characterization and photoluminescence

We have synthesized ZnS nanowires with mane-like branches by thermal evaporation of ZnS powder on the Au-coated Si(100) substrate using a two-heating zone tube furnace. The ZnS powder and the Si substrate were kept at 1,000 and 850 °C, respectively, in a nitrogen atmosphere during synthesis of the ZnS nanostructures. Field emission scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction, and photoluminescence (PL) spectroscopy analyses were performed to investigate the structure, morphology and photoluminescence properties of the products. The axial nanowires grow along the [002] direction and have diameters of 100–200 nm, while on the other hand the branch nanowires grow along the [101] direction and their diameters and lengths are 30–50 and 800–100 nm, respectively. The room temperature PL spectrum with a Gaussian fitting exhibits two visible light emission bands centered at around 397 and 458 nm.     

Inverted organic solar cells with ZnO nanowalls prepared using wet chemical etching in a KOH solution

We report on the photovoltaic (PV) performances of inverted organic solar cells (IOSCs) that were fabricated from PCBM:P3HT polymer with a ZnO thin film and ZnO nanowalls as electron transport and hole block layers. ZnO thin film on ITO/glass substrate was deposited using a simply aqueous solution route. ZnO nanowall structures were obtained via wet chemical etching of ZnO thin films in a KOH solution. The power conversion efficiency (PCE) of the IOSC with ZnO nanowalls was significantly improved by 44% from 1.254% to 1.811% compared to that of the IOSC with ZnO thin film. The short circuit current in IOSCs fabricated with the ZnO nanowalls was increased mainly due to the increase in the charge transport interface area, as a result of enhancement in the PCE. This work suggests a method for fabricating efficient PV devices with a larger charge transport area for future prospects.     

Synthesis and characterization of carbon/silica superhydrophobic multi-layer films

C/SiO₂ multi-layer films (3-layer films and 5-layer films) were obtained by sol-gel method and physical deposition on glass plates, and then heated at 500 °C for 1 h under a nitrogen atmosphere. The mechanical adhesive force with the substrate of the multi-layer films was sharply enhanced compared to the as-deposited amorphous carbon film. An absorption layer was formed on heat treated C/SiO₂ multi-layer films by modification of the surface with trimethylchlorosilane, and the wettability of the films changed from hydrophilic to super-hydrophobic. The structures of the physically deposited carbon and the multi-layer films were analyzed by X-ray diffraction, transmission electron microscopy and scanning electron microscopy. The experimental results showed that the 5-layer films had a concentric ring structure that caused the film to be superhydrophobic.