Preparation and microwave absorption properties of electroless Co-P-coated nickel hollow spheres

Co-P-coated nickel hollow spheres (NHSs) were prepared by electroless plating technology. The morphology and component content of Co-P coating varies with the change of sodium citrate concentration in elctroless plating solution. And as phosphorus content increases in coatings, resulting in smaller grain, coercivity of microspheres decreases. The microwave absorption properties of spheres-wax composite were investigated in the range of 2-18 GHz. Both permittivity and permeability increase with an increase of cobalt content in coatings. For composite layer, a minimal reflection loss (RL, −36.9 dB) of was predicted at 8.1 GHz with a thickness of 3 mm.     

Electromagnetic and microwave absorption properties of Fe3O4 magnetic films plated on hollow glass spheres

Magnetic hollow spheres of low density were prepared by plating Fe₃O₄ magnetic films on hollow glass spheres using ferrite plating. The complex permeability and permittivity of spheres–wax composites were measured in the range of 2–18 GHz. The complex permeability and permittivity increased, and the dielectric and magnetic losses were improved as the volume fraction of the magnetic spheres in the composites increased from 60% to 80%, which also resulted in a great improvement of microwave absorption properties. For composites with volume fraction 80%, its magnetic resonance frequency was at about 13 GHz and it appeared three loss peaks in the calculated reflection loss curves; the bandwidth less than −10 dB was almost 4 GHz which was just in the Ku-band frequencies (12–18 GHz) and a minimum reflection loss of −20 dB was obtained when the thickness was 2.6 mm; the microwave absorbing properties were mainly due to the magnetic loss. The results showed that the magnetic spheres composites were good and light microwave absorbers in the Ku-band frequencies.     

A self-generated template route to hollow carbon nanospheres in a short time

A self-generated template route was reported to prepare hollow carbon nanospheres. The hollow spheres were obtained through the direct pyrolysis of ferrocene for 1 h. The external diameter of the hollow carbon nanospheres was 50-150 nm and the thickness of the wall was about 15 nm. A possible formation mechanism of the hollow carbon nanospheres was discussed.     

Synthesis, characterization and photodegradation study of mixed-phase titania hollow submicrospheres with rough surface

Titania hollow submicrospheres with mixed phase (anatase-brookite or anatase-rutile) were synthesized via the combination of hydrothermal treatment and calcination of submicrospheres consisting of a polystyrene core and an amorphous TiO₂ shell. After hydrothermal treatment, amorphous titania shell could be transformed to anatase-brookite shell consisting of loose packed titania nanocrystals, which could be further converted to anatase-brookite (below 700 °C) or anatase-rutile titania (700-800 °C) hollow spheres with rough surface via calcination. The loose packing of titania nanocrystals not only inhibited the transformation temperature from anatase to rutile, but also provided titania hollow submicrospheres with high photodegradation activity of Rhodamine B. The photocatalytic activity of titania hollow spheres increased firstly then decreased when the calcination temperature was varied in the range of 450-800 °C, while hollow spheres obtained via calcinating at 700 °C exhibited the highest photocatalytic activity, which was five times higher than that of counterpart without hydrothermal treatment.     

Preparation of titania hollow spheres by catalyst-free hydrothermal method and their high thermal stabilities

TiO₂ hollow spheres have been prepared by hydrothermal method using carbon spheres as hard templates based on template-directed deposition and calcination in order to remove templates. The morphology and structure of samples were systematically characterized by using various techniques, including XRD, zeta analyzer, SEM, TEM, DRS and FTIR. In this approach, the anatase phase was retained for temperatures up to 900 °C. Moreover, negative charged titania is deposited onto the negative charged surface of carbon spheres, which is proved by nanoparticle size analyzer. Therefore, a possible formation mechanism of TiO₂ hollow spheres was proposed. TiO₂ hollow spheres calcined at 550 °C exhibited the superior photocatalytic activity for the degradation of Rhodamine B, 2.9 times greater than that of Degussa P25. Furthermore, thermal stability of TiO₂ hollow spheres was examined. Fortunately, we found that hollow structures could still be visible distinctly after calcining at 900 °C.     

Study on the surface erosion route to the fabrication of TiO2 hollow spheres

Three-dimensional (3D) architecture of TiO₂ hollow sphere has many excellent and interesting performances that attract significant attention nowadays. In this paper, a simple surface erosion approach to the fabrication of TiO₂ hollow spheres via the hydrothermal process has been developed. The morphologies and the phase were characterized by scanning electron microscopy (SEM) and X-ray diffractometer (XRD). The results indicate that the anatase-type TiO₂ hollow spheres with a diameter of ∼1 μm are successfully synthesized. The shell thickness of TiO₂ hollow spheres is ∼150 nm and the size of hollow cavity is ∼600 nm. By the control experiments, the influence of ammonium fluoride and hydrogen peroxide on the hollow spherical structures was studied. Hydrogen peroxide acts as both the oxidant and the bubble generator, ammonium fluoride is crucial for the erosion and dissolution of titanium, the detailed dissolution-crystallization mechanism for the formation of TiO₂ hollow spheres was also proposed.     

Synthesis of hollow ferrite nanospheres for biomedical applications

Hollow ferrite spheres of 220-340 nm diameter were synthesized at 60 °C as multi-functionalized magnetic carriers which are potentially applicable both as drug delivery systems (DDS) and hyperthermia treatment. We found that SH and OH groups on the silica template spheres enabled the fabrication of continuous ferrite shells of 20-30 nm in thickness. Transmission electron microscopy and energy-dispersive spectroscopy revealed that the templates were dissolved by a NaOH solution, yielding hollow particles exhibiting saturation magnetization of 78 emu/g. The results suggested that the ferrite shells are porous and the pores work as pathway for releasing drugs from the hollow particle inside.     

Synthesis of porous hollow silica spheres using polystyrene-methyl acrylic acid latex template at different temperatures

Porous hollow silica spheres were prepared by using polystyrene-methyl acrylic acid latex as a template and cetyltrimethylammonium bromide as a wall structure-directing agent starting from tetraethoxysilane. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), FT-infrared spectroscopy (FT-IR) and nitrogen adsorption/desorption were used to characterize the hollow silica spheres. When silica-coated latex composites were prepared at room temperature, hollow silica spheres with micropores in the walls were formed after removing the latex templates by calcination. When silica-coated latex composites were aged at a higher temperature of 150 °C, intact mesoporous hollow silica spheres were formed after calcination treatment.     

Facile synthesis and characterization of glass/cobalt core/shell composite spheres with tunable shell morphologies

Polyhedral cobalt microcrystals assembled on hollow glass spheres are successfully synthesized by a facile and easy-control hydrothermal reduction process, and thus hierarchical glass/cobalt core/shell composite hollow spheres are fabricated with low-density (0.96 g cm⁻³). By properly tuning the process conditions and the component of the reaction solution, a series of composite spheres with gradient in morphologies of the shell layer can be prepared. Based on a series of contrast experiments, the probable formation mechanism of the core/shell hierarchical structures is proposed. The magnetic properties of the products are studied and the results demonstrate that the composite spheres present ferromagnetic properties related to the special shell morphologies. The composite hollow spheres thus obtained may have some promising applications in the fields of low-density magnetic materials, conduction, and catalysis, etc. This work provides an additional strategy to prepared core/shell composite spheres with tailored shell morphology and magnetic properties.     

A room-temperature approach to boron nitride hollow spheres

Boron nitride hollow spheres were synthesized by the reaction of BBr₃ and NaNH₂ at room temperature; X-ray powder diffraction pattern could be indexed as hexagonal BN with the lattice constants of a=2.482 and c=6.701 Å; high-resolution transmission electron microscopy image showed the hollow spheres consisted of BN nanoparticles, with diameter between 80 and 300 nm; a possible formation mechanism of BN hollow spheres was discussed.     

Nano-sized silica hollow spheres: Preparation, mechanism analysis and its water retention property

In this article, synthesis of nano-sized silica hollow spheres applying positive charged polystyrene as sacrificial templates was introduced. Firstly, nano-sized polystyrene particles were synthesized by emulsifier-free emulsion polymerization under solvothermal condition. Secondly, silica hollow nanospheres were formed through a simultaneous ‘coating-etching’ process. PVP played a key role in the evolution of nano-sized hollow spheres even if the templates were positive charged and the formation mechanism was different from that of previous studies. TEM results revealed that the morphologies of nano-sized silica hollow spheres not only strongly relied on the amount of reactant, but also the sequence of adding them. TGA illustrated that the interiors of nano-sized silica hollow spheres were not completely ‘hollow’. Brunauer-Emmett-Teller (BET) analysis showed that this material had a specific area of 399 m²/g. The water retention property of the materials was also investigated.     

Synthesis of hollow silver spheres using poly-(styrene-methyl acrylic acid) as templates in the presence of sodium polyacrylate

Hollow silver spheres were successfully prepared by reducing AgNO₃ with ascorbic acid and using negatively charged poly-(styrene-methyl acrylic acid) (PSA) spheres as templates in the presence of sodium polyacrylate as a stabilizer. Firstly, silver cations adsorbed on the surface of PSA spheres via electrostatic attraction between the carboxyl groups and silver cations were reduced in situ by ascorbic acid. The silver nanoparticles deposited on the surface of PSA spheres served as seeds for the further growth of silver shells. After that, extra amount of AgNO₃ and ascorbic acid solutions were added to form PSA/Ag composites with thick silver shells. In order to obtain compact silver shells, the as-prepared PSA/Ag composites were heated at 150 °C for 3 h. Then hollow silver spheres were prepared by dissolving PSA templates with tetrahydrofuran.     

Room temperature preparation of cuprous oxide hollow microspheres by a facile wet-chemical approach

Cuprous oxide hollow spheres have potential applications in drug-delivery carriers, biomedical diagnosis agents, and cell imaging. From a commercial point of view, the low-temperature, template-free, facile method is widely popular synthetic method for the synthesis of cuprous oxide hollow spheres. In this letter, we describe a novel facile template-free wet-chemical route to prepare crystallized cuprous oxide microspheres at room temperature. XRD patterns and SEM images revealed that pure crystallized cuprous oxide hollow microspheres were successfully obtained at room temperature. The diameter of cuprous oxide hollow sphere can be adjusted (0.7-7 μm) by concentration control of hydrazine hydrate. Generated N₂ gas bubbles in the aqueous solution, serving as “soft” templates, play a key role in the formation of hollow microspheres.     

Synthesis and characterizations of spherical hollow composed of AgI nanoparticle using AgBr as the precursor

Hollow spheres of AgI with an average radius of 100-200 nm have been prepared by a simple reaction between AgBr suspension and KI in the presence of gelatin. Gelatin played a decisive role as an inhibitor of the direct attack of I⁻ ions to AgBr surfaces and coagulation of the growing AgI in producing the spherical AgI particles. The products were characterized by X-ray powder diffraction, transmission electron microscopy, UV-vis absorption spectroscopy and X-ray photoelectron spectra techniques. The band gaps are estimated to be 2.95 eV according to the results of optical measurements of the hollow spheres of AgI.     

Potato starch-based activated carbon spheres as electrode material for electrochemical capacitor

Potato starch-based activated carbon spheres (PACS) were prepared from potato starch by stabilization, carbonization followed by activation with KOH. The obtained PACS are hollow and retain the original morphology of potato starch with decrease in size, as shown by scanning electron microscopy. Modification of textural properties of the PACS was achieved by varying the carbonization temperature and the ratio of KOH/PCS. The results of N₂ adsorption isotherms indicate that the samples prepared are mainly microporous. The electrochemical behaviors of the hollow PACS were studied by galvanostatic charge-discharge, cyclic voltammetry, and impedance spectroscopy. The results indicate that high specific capacitance of 335 F/g is obtained at current density 50 mA/g for PACS with specific surface area 2342 m²/g. Only a slight decrease in capacitance, to 314 F/g, was observed when the current density increases to 1000 mA/g, indicating a stable electrochemical property.     

Preparation, characterization and photocatalytic activity of the neodymium-doped TiO2 hollow spheres

Nd-doped titania hollow spheres were prepared using carbon spheres as template and Nd-doped titania nanoparticles as building blocks. The Nd-doped titania nanoparticles were synthesized at low temperature. The prepared hollow spheres were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), scanning electron microscope (SEM), X-ray photoelectron spectroscopy (XPS) and UV-vis diffuse reflectance spectrum (DRS). The effects of Nd content on the physical structure and photocatalytic activities of doped titania hollow sphere samples were investigated. Results showed that there was an optimal Nd-doped content (3.9 at.%) for the photocatalytic degradation of dye X-3B (C.I. Reactive Red 2). The apparent rate constant of the best one was almost 9 times as that of P25 titania. The mechanism of photocatalytic degradation of dyes under visible light irradiation was also discussed.     

Self-assembled MnS flower-like hierarchical architectures on porous alumina membrane

MnS flower-like hierarchical architectures were self-assembled on the surface of porous alumina membrane (PAM) under hydrothermal condition. The diameter of MnS flower-like hierarchical architectures is about 2-4 μm, which are composed of single-crystal nanowires with width of 70-80 nm. X-ray diffraction and high-resolution transmission electron microscopy analysis demonstrated the nanowire have preferred orientation along [1 1 0] direction. Prolonged reaction time would result in hollow spheres. Studies show that PAM and gas bubbles formed within the nanopores of PAM under hydrothermal condition play an important role in the formation process of MnS flower-like hierarchical architectures. The room-temperature PL spectrum shows a strong emission peak at 420 nm corresponding to the MnS band edge emission.     

Large-quantity synthesis of ZnO hollow objects by thermal evaporation: Growth mechanism, structural and optical properties

Synthesis of large-quantity uniformly distributed ZnO hollow objects, i.e. cages and spheres have been performed on Si(1 0 0) and steel alloy substrates by the direct heating of metallic zinc powder in the presence of oxygen. Extensive structural observations revealed that the formed products are crystalline ZnO with the wurtzite hexagonal phases. The Raman-active optical phonon E₂ modes, attributed to wurtzite hexagonal phase of ZnO, were observed at 437 cm⁻¹ for the products grown on both the substrates. The room-temperature photoluminescence spectra showed a broad band in the visible region with a suppressed UV emission, indicating the presence of oxygen vacancies and structural defects in the as-grown structures. Additionally, post growth annealing was also carried out to further investigate the photoluminescence properties of the as-grown products. It was observed that the formation of hollow objects consists of several stages which include the formation of Zn clusters, oxidation on the sheath and sublimation/evaporation of the Zn from the interiors, resulted in the formation of hollow objects.     

Preparation and microwave absorption properties of loose nanoscale Fe3O4 spheres

Magnetite nanoparticles are found to assemble into randomly dispersed loose nanoscale spheres with diameters ∼300 nm in ethylene glycol in the presence of polyethylene and a small quantity of polyethyleneimine. Modern analysis methods are employed to provide structure information of the magnetic loose spheres. The ferromagnetic saturation magnetization is ∼80.0 emu g⁻¹, and the coercive force is 209 Oe. The microwave electromagnetic parameters are measured by a vector network analyzer. The synthesized loose spheres exhibit novel microwave properties compared with the conventional Fe₃O₄ nanoparticles. An additional microwave loss peak appears in the Ku band, which is attributed to the loose structure.     

Preparation and optical properties of Cu2O hollow microsphere film and hollow nanosphere powder via a simple liquid reduction approach

In this work, we report a simple liquid reduction approach to prepare Cu₂O hollow microsphere film and hollow nanosphere powder with Cu(OH)₂ nanorods as precursor and ascorbic acid as the reductant at 60 °C. When Cu(OH)₂ nanorod array film grown on a copper foil is used as the precursor, Cu₂O thin film made up of hollow microspheres with average diameter of 1.2 μm is successfully prepared. When the Cu(OH)₂ nanorods are scraped from the copper foil and then used as the precursor, Cu₂O hollow nanosphere powder with the average diameter of 270 nm is obtained. The samples are characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and ultraviolet-vis light (UV-vis) absorption spectra. A possible formation mechanism of Cu₂O hollow spheres is discussed.