Rapid synthesis of TiO2 hollow nanostructures with crystallized walls by using CuO as template and microwave heating

In this paper, TiO₂ hollow nanostructures with anatase walls have been rapidly fabricated by using CuO as template and microwave heating. These TiO₂ hollow nanostructures have been characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). Experimental results showed that the TiO₂ shell transformed from amorphous to anatase phase in 3 min, induced by the hot CuO core under microwave irradiation. The diameter of TiO₂ hollow nanostructures is about 50-80 nm, and the length is about 200-300 nm. The thickness of the shell is about 3 nm. This method is promising to be used to synthesize other nanomaterials with a hollow nanostructure.     

Synthesis and characterization of CuO nanowhiskers by a novel one-step, solid-state reaction in the presence of a nonionic surfactant

A novel and simple one-step, solid-state reaction in the presence of a nonionic surfactant, PEG 400, has been developed to synthesize CuO nanowhiskers with diameters of approximately 2-10 nm and lengths of more than 100 nm. The CuO nanowhiskers were characterized by XRD, TEM, HRTEM and XPS.     

Sol-gel synthesis of titania hollow spheres

TiO₂ hollow spheres are prepared by a convenient sol-gel method at room temperature. The products were characterized by XRD, FESEM, TEM and FT-IR. It was found that these spheres are hollow inside with outer diameters of 200-500 nm. The average mesoporous diameter is about 9.8 nm. And the BET surface area and specific pore volume are about 161.9 m²/g and 0.441 cm³/g, respectively.     

Syntheses and gas-sensing properties of CuO nanostructures by using [Cu(pbbt)Cl2]2·CH3OH as a precursor

The rod-like and dandelion-like CuO nanomaterials have been prepared by the decomposition of a copper complex [Cu(pbbt)Cl₂]₂·CH₃OH (pbbt = 1,1′-(1,3-propylene)-bis-1H-benzotriazole) in the presence of suitable surfactants and alkalies under hydrothermal conditions. The CuO nanorods are about 50 nm in diameter and up to 500-700 nm in length; the average diameter of the dandelion-like CuO microspheres is of 2 μm. A formation mechanism for the CuO nanomaterial was proposed. The gas-sensing properties of as-prepared CuO nanomaterial were studied. The sensitivity of the as-prepared CuO nanorods was better than that of dandelion-like CuO particles, and the CuO nanorods displayed special sensitivity to alcohol.     

Ultrasound assisted template-free synthesis of Cu(OH)2 and hierarchical CuO nanowires from Cu7Cl4(OH)10·H2O

Cu(OH)₂ nanowires have been synthesized by an ultrasound assisted solution route in absence of a template, using Cu₇Cl₄(OH)₁₀·H₂O as a precursor. Hierarchical CuO nanowires were obtained by a simple solid-state thermal transformation of these Cu(OH)₂ nanowires. The products were characterized by XRD, SEM, TEM and HRTEM. The ranges of diameters and lengths of the polycrystalline CuO nanowires are ca. 20-30 nm and several micrometers, respectively. Ultrasonic time is found an important factor to morphology of the CuO products. This could be a potential efficient way for large scale fabrication of CuO nanowires with hierarchical structures. Surface photovoltage spectra of the CuO nanowires in air, NH₃ and CH₂Cl₂ atmospheres were investigated, which demonstrates it a good photoelectric gas sensing material.     

Novel MoO3 and WO3 hollow nanospheres assembled with polymeric micelles

Novel β-MoO₃ and WO₃ hollow nanospheres were synthesized using a soft template of polymeric micelle with core-shell-corona architecture. Poly(styrene-b-[3-(methacryloylamino)propyl] trimethylammonium chloride-b-ethylene oxide) micelles (PS-PMAPTAC-PEO) with cationic shell block effectively produce core/shell composite particles through electrostatic interaction with anionic precursors WO₄²⁻ and MoO₄²⁻. Transmission electron microscope (TEM) images of β-MoO₃ and WO₃ have confirmed the hollow structure with average outer diameter of 42 ± 2 and 46 ± 2 nm, respectively; the hollow cavity diameters were found to be 16  ± 1 nm and 14 ± 1 nm for β-MoO₃ and WO₃, respectively. The combination of nitrogen adsorption/desorption analyses and TEM observation confirmed the presence of disordered mesopores in the shell domain of β-MoO₃ and WO₃ hollow particles.     

Solvothermal synthesis of the special shape (deformable) hollow g-C3N4 nanospheres

Special shaped (deformable) hollow g-C₃N₄ nanospheres were synthesized by the solvothermal technique using silica spheres as template. The X-ray diffraction (XRD) peaks of the product were indexed to g-C₃N₄ materials. Field-Emission Scanning Electron Microscopy and Transmission Electron Microscopy confirmed that the external diameter of the hollow nanospheres is about 130-150 nm and thickness of the wall is about 20-30 nm. The FTIR spectrum showed absorption peak at 810 cm^-1 can be attributed to the s-triazine (C₃N₃) breathing mode. Raman spectrum exhibited two broad peaks approximately at 1360 cm^-1 (D band) and 1580 cm^-1 (G band). The deformed pie shape or mortars like hollow spheres were first reported. The flexility of the deformable hollow g-C₃N₄ nanospheres may be used in special field such as drug delivery carriers adjusting the delivery ratio by the external pressure, and a good material for studying the mechanical properties of the sp² hybrid g-C₃N₄. The photoluminescence spectrum of the product indicates that the deformable hollow g-C₃N₄ nanospheres may have potential applications in nano-optical device fields.     

Solvo-solid preparation of Zn3N2 hollow structures; their PL yellow emission and hydrogen absorption characteristics

Zinc nitride (Zn₃N₂) hollow structures with 10-25 μm size have been prepared by solvo-solid approach using aqueous ammonia treated Zn precursor at reaction temperature of 600 °C for reaction time of 240 min under ammonia gas flow. The structural, compositional and morphological characterizations of the as-obtained product were performed by XRD, EDS and SEM. Room temperature photoluminescence (PL) spectrum of zinc nitride hollow structures (ZNHSs) exhibited UV emission band at 384 nm and a defect related yellow emission band at 605 nm. The first ever studies on hydrogen absorption characteristics of ZNHSs performed at 373 K showed an absorption capacity of 1.29 wt.%. Growth mechanism proposed for the formation of ZNHSs is also discussed briefly.     

Direct synthesis and characterization of spongy CuO with nanosheets from Cu3(btc)2 microporous metal-organic framework

Spongy CuO was successfully synthesized via direct pyrolysis of Cu₃(btc)₂ (btc = benzene-1,3,5-tricarboxylate) microporous metal-organic framework (MOF) in a horizontal tube furnace in the air, in which the Cu₃(btc)₂ was used as the Cu source and complexing molecule precursor. The as-prepared products were characterized by a series of techniques including XRD, SEM, EDX, TEM, and SAED. Results from SEM showed that the as-prepared spongy CuO with average diameter altering from 10 to 20 μm consists of nanosheets with average edge length in the range of 80-200 nm and thickness of about 30 nm, which was also confirmed by TEM analysis. The XRD and SAED results showed that a purity phase of CuO was obtained after pyrolysis. It was also found that the reaction temperature played a key role in the formation of spongy CuO microstructures. The spongy material could be found potential application in various fields such as catalysis, absorption, and gas sensing.     

CuO microflowers composed of nanosheets: Synthesis, characterization, and formation mechanism

CuO microflowers composed of nanosheets with tunable size have been fabricated through a simple reaction in ammonia solution at 90-180 °C, in which the nanosheets with zigzag edges were 20-40 nm in thickness and 500-800 nm in width. The high ammonia concentration, high ratio of CNH₃ to CCu2+ (R_ac) and elevated temperature were necessary for the formation of microflowers, and the ammonia concentration was critical for the morphology evolution of the particles. The fabrication mechanism of CuO microflowers based on the assembly of Cu(OH)₂ nanobelts was discussed. In addition, the CuO microflowers showed effective catalytic activity on the decomposition of ammonium perchlorate.     

Influences of refrigerant-based nanofluid composition and heating condition on the migration of nanoparticles during pool boiling. Part I: Experimental measurement

Influences of refrigerant-based nanofluid composition and heating condition on the migration of nanoparticles during pool boiling were investigated experimentally. The nanoparticles include Cu (average diameters of 20, 50 and 80 nm), Al and Al₂O₃ (average diameters of 20 nm), and CuO (average diameter of 40 nm). The refrigerants include R113, R141b and n-pentane. The mass fraction of lubricating oil RB68EP is from 0 to 10 wt%, the heat flux is from 10 to 100 kW m⁻², and the initial liquid-level height is from 1.3 to 3.4 cm. The experimental results show that the migration ratio of nanoparticles during the pool boiling of refrigerant-based nanofluid increases with the decrease of nanoparticle density, nanoparticle size, dynamic viscosity of refrigerant, mass fraction of lubricating oil or heat flux; while increases with the increase of liquid-phase density of refrigerant or initial liquid-level height.     

Characteristics of Eu-doped Ca-α-SiAlON phosphor powders prepared by spray pyrolysis process

Eu²⁺-doped Ca-α-SiAlON phosphor powders with fine size and regular morphology were prepared by combining spray pyrolysis and the carbothermal reduction and nitridation processes. The precursor powders were prepared by spray pyrolysis from the spray solution with ethylenediaminetetraacetic acid, citric acid, and sucrose; they had large sizes, were hollow, and had thin wall structures. The precursor powders containing a carbon component turned into Ca-α-SiAlON phosphor powders after firing at 1450 °C under a H₂/N₂ mixture gas. The mean size of the phosphor powders was 5.1 μm. The phosphor powders had a broad excitation spectra range of 250-500 nm; this consisted of two broadbands centered at 305 and 400 nm. When excited by a 455-nm blue light, the emission spectra of the phosphor powders displayed a broadband in the range of 500-700 nm, which resulted in a yellow emission. The wavelength of the emission spectrum showing the maximum intensity was 576 nm.     

Hydrogen peroxide-assisted hydrothermal synthesis of hierarchical CuO flower-like nanostructures

Hierarchical CuO nanostructures were synthesized through a hydrogen peroxide-assisted hydrothermal route in which Cu(OH)₂ was the copper source. The CuO nanostructures were composed of numerous nanobelts that radiated from the center of the nanostructure and formed a flower-like shape with a diameter of 5-10 μm. The nanobelts had lengths of 2.5-5 μm and widths of 150-200 nm. The H₂O₂ concentration directly influenced the product morphology. As the concentration of H₂O₂ increased, the length and width of the nanobelts increased and the quantity of the nanobelts decreased. The possible formation mechanism of hierarchical CuO flower-like nanostructures was presented.     

Facile template-free sonochemical fabrication of hollow ZnO spherical structures

ZnO hollow spherical structures have been synthesized by a facile template-free sonochemical process. The structures and morphologies of products have been characterized by XRD, FESEM and TEM. The results reveal that hollow spherical structures possess a hexagonal wurtzite structure with the in- and out-diameters of about 400 and 500 nm, respectively. The walls of the hollow structures are self-assembled by nanoparticles, partly composed of hexagonal nanoflakes with 40 nm in side lengths. Room temperature photoluminescence (PL) spectrum showed a UV emission at ∼ 384 nm and a broad green emission at the center of 535 nm. A possible formation mechanism was also proposed.     

Synthesis and characterization of large area well-aligned carbon nanotubes by ECR-CVD without substrate bias

Large area, well-aligned carbon nanotubes (CNTs) were synthesized on porous silicon by electron cyclotron resonance chemical vapor deposition (ECR-CVD). No bias was applied on the substrate in this experiment. CH₄ and H₂ were used as source gases and Fe₃O₄ nanoparticles as the catalyst. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction spectroscopy (XRD), and Raman spectrum were used to evaluate the structure and composition. The results show that these CNTs have varying outer diameters from 10 to 90 nm and uniform length over 10 μm. They display hollow tubular and chain structures. The possible formation mechanism of aligned CNTs is discussed.     

Synthesis of nano-TiC powder using titanium gel precursor and carbon particles

The paper presents a novel process for synthesis of nano-size titanium carbide by reaction between titanium bearing precursor gel and nano carbon particles derived from soot at different temperatures in the range of 1300-1580 °C for 2 h under argon cover. The HRTEM studies of TiC powder synthesized by heating at 1580 °C show the presence of cube shaped particles (~ 60-140 nm) and hollow rods (diameter ~ 30-185 nm). The average particle size of crystallites, calculated by Scherer equation is observed to be ~ 35 nm while the surface area-density measurements indicate it to be ~ 113 nm. The surface area decreases with increase in reaction temperature.     

Hierarchically nanostructured Fe3O4 microspheres and their novel microwave electromagnetic properties

Magnetite nanoparticles are found to assemble into monodisperse Fe₃O₄ microspheres with diameters ∼ 300 nm and open pores on the shells in ethylene glycol (EG) in the presence of polyethylene 2000 (PEG 2000) and a small quantity of polyethyleneimine (PEI). The hysteresis loops of the magnetic microspheres are measured by a vibrating sample magnetometer (VSM), the ferromagnetic signature emerged with the saturated magnetization of ∼ 80.0 emu g^− 1, and the coercive force of ∼ 208.7 Oe. The synthesized hierarchical microspheres exhibit two microwave magnetic loss peaks: one appears at 4.0-5.0 GHz, the other appears around 16.0-17.0 GHz. The latter peak is attributed to the effect of the morphology of the hierarchical structure. Modern analysis methods SEM, TEM, XRD etc., are employed to figure the detailed structure information of the magnetic hollow spheres.     

Self-template route to MnO2 hollow structures for supercapacitors

Birnessite-type MnO₂ hierarchical hollow structures were prepared through a self-template route, by the direct reaction between the aqueous solution of KMnO₄ and solid MnCO₃ precursor crystals, and followed by the removal of MnCO₃ core with HCl. Field emission scanning microscopy (FESEM) images indicate that the shells of hierarchical hollow structures consist of the interconnected sheets with a thickness of about 30 nm, and transmission electron microscopy (TEM) images show that the thickness of the shells can be adjusted over a range from 50 to 80 nm by changing the molar ratio of MnCO₃/KMnO₄. The electrochemical properties of the as-prepared MnO₂ were characterized by cyclic voltammetry (CV) and galvanostatic charge-discharge tests in 1 M Na₂SO₄ solution. The sample obtained at a higher MnCO₃/KMnO₄ molar ratio (i.e., 50:1) shows a relatively higher specific capacitance of 169 F g^− 1 than 111 F g^− 1 of the sample obtained under a lower molar ratio of 25:1 at the current density of 250 mA g^− 1.     

Template-free synthesis of SnO2 nanostructural hollow spheres covered by nanorods

In the present work, SnO₂ nanostructural hollow spheres have been successfully synthesized in the absence of template by a simple synthetic route, and their surfaces were covered by nanorods. The synthesized nanostructural hollow spheres covered by nanorods were further characterized by XRD, SEM and TEM measurements. The diameter of SnO₂ hollow spheres and the thickness of shells are found to be ca. 150-200 and 20-30 nm, respectively. The size of the nanorod is found to be ca. 5 nm, and the length up to tens of nanometers. Based on a series of experimental results, an oxidizing-aggregating-Ostwald ripening model has been proposed for the formation of SnO₂ nanostructural hollow spheres.     

Synthesis of nanometal oxides and nanometals using hot-wire and thermal CVD

We report the synthesis of nano-oxides of molybdenum, tungsten, and zinc. Molybdenum oxide (MoO₃) and tungsten oxide (WO_x) were produced by hot-wire CVD with molybdenum and tungsten filaments, respectively while zinc oxide (ZnO) was produced by thermal CVD. When high purity molybdenum wire was oxidized at ambient system atmosphere, nanorods and nanostraws of MoO₃ with length ranging from ∼ 20-80 nm and diameters ranging from ∼ 5-15 nm were produced. Also, the oxidation of the tungsten filament led to the deposition of tungsten oxide nanorods (10-25 nm diameter and 75-90 nm long) and nanospheres with diameters of ∼ 60 nm. Each oxide was reduced to its metallic form by annealing in a hydrogen environment to produce metallic nanoparticles. Nanorods and nanoribbons of ZnO with diameters ranging from 20-65 nm and lengths up to 2 μm were also produced.