PVP Assisted Shape-Controlled Synthesis of Self-Assembled 1D ZnO and 3D CuO Nanostructures

Self-assembled one-dimensional (1D) zinc oxide (ZnO) rods and three-dimensional (3D) cupric oxide (CuO) cubes like nanostructures with a mean crystallite size of approximately 33 and 32 nm were synthesized through chemical route in the presence of polyvinylpyrrolidone (PVP) under mild synthesis conditions. The technique used for the synthesis of nanoparticles seems to be an efficient, inexpensive and easy method. X-Ray diffraction patterns confirmed well crystallinity and phase purity of the as prepared samples, followed by the compositional investigation using Fourier Transform Infrared (FT-IR) spectroscopy. The formation of ZnO nanorods and CuO nanocubes like structures were through Scanning Electron Microscopy (SEM) images. The mechanism and the formation factors of the self-assembly were discussed in detail. It was clearly observed from results that the concentration of precursors and PVP were important factors in the synthesis of self-assembly ZnO and CuO nanostructures. These self-assembly nanostructures maybe used as novel materials in various potential applications.     

Utilization of ultrasonic irradiation as a green and effective strategy to prepare poly(N-vinyl-2-pyrrolidone)/modified nano-copper (II) oxide nanocomposites

The present paper describes the result of investigations into preparation of novel nanocomposites (NCs) based on poly(N-vinyl-2-pyrrolidone) (PVP) as a biocompatible polymer and modified copper (II) oxide nanoparticles (NPs) as a nano-filler. To achieve optimum NCs properties, different ratios of modified copper (II) oxide NPs (3, 5, and 7 wt%) were used to fabricate PVP NCs and also the ultrasonic irradiation was utilized to perform these processes as a fast and effective method. Subsequently, the structure of the obtained nanohybrids was characterized by various techniques. The suitable incorporation between PVP matrix and modified CuO NPs can be seen from the FT-IR spectra. The obtained NCs indicated an efficient thermal improvement in comparison to the pristine polymer. Also, the uniform dispersion of modified CuO NPs in the PVP matrix was detected by FE-SEM and EDX. According to UV absorption spectra, it is clear that these NCs can be used in UV protecting applications.     

Syntheses and characterization of Mg(OH)2 and MgO nanostructures by ultrasonic method

Magnesium hydroxide nanostructures have been synthesized by the reaction of magnesium acetate with sodium hydroxide via sonochemical method. Reaction conditions such as the Mg²⁺ concentration, aging time and the ultrasonic device power show important roles in the size, morphology and growth process of the final products. The magnesium oxide nanoparticles have been prepared by calcination of magnesium hydroxide nanostructures at 400 °C. The magnesium hydroxide and magnesium oxide nanostructures were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), thermal gravimetric (TG) and differential thermal analyses (DTA).     

Sonochemical synthesis and characterization of lead iodide hydroxide micro/nanostructures

For the first time, micro/nano-sized lead iodide hydroxide; Pb(OH)I, has been successfully prepared via a simple ultrasonic method. In this method, lead nitrate and lithium iodide were applied as starting reagents to fabricate Pb(OH)I micro/nanostructures at different conditions. The effect of different surfactants like N,N-bis(salicylidene)-ethylenediamine (H₂salen), sodium dodecyl sulfate (SDS) and polyvinylpyrrolidone (PVP), sonication time, and ultrasonic intensity on the morphology and particle size of the products has been investigated. The as-produced micro/nanostructures were characterized with the aid of XRD, SEM, TEM, UV–vis, EDS and FT-IR. According to the SEM images, different morphologies of Pb(OH)I including micro- and nano-sized rods were formed by changing the preparation conditions. Based on the XRD results, it was found that Pb(OH)I and PbI₂ have been produced with and without sonication at the same conditions, respectively. The use of the H₂salen and sonication treatment were confirmed to be the crucial factors determining the formation of one-dimensional Pb(OH)I micro/nanostructures.     

Characterization of nanostructured CuO–porous silicon matrix formed on copper-coated silicon substrate via electrochemical etching

A pulsed anodic etching method has been utilized for nanostructuring of a copper-coated p-type (100) silicon substrate, using HF-based solution as electrolyte. Scanning electron microscopy reveals the formation of a nanostructured matrix that consists of island-like textures with nanosize grains grown onto fiber-like columnar structures separated with etch pits of grooved porous structures. Spatial micro-Raman scattering analysis indicates that the island-like texture is composed of single-phase cupric oxide (CuO) nanocrystals, while the grooved porous structure is barely related to formation of porous silicon (PS). X-ray diffraction shows that both the grown CuO nanostructures and the etched silicon layer have the same preferred (220) orientation. Chemical composition obtained by means of X-ray photoelectron spectroscopic (XPS) analysis confirms the presence of the single-phase CuO on the surface of the patterned CuO–PS matrix. As compared to PS formed on the bare silicon substrate, the room-temperature photoluminescence (PL) from the CuO–PS matrix exhibits an additional weak ‘blue’ PL band as well as a blue shift in the PL band of PS (S-band). This has been revealed from XPS analysis to be associated with the enhancement in the SiO₂ content as well as formation of the carbonyl group on the surface in the case of the CuO–PS matrix.     

Versatile synthesis of rectangular shaped nanobat-like CuO nanostructures by hydrothermal method; structural properties and growth mechanism

This paper describes a simple and versatile method for growing highly anisotropic rectangular shaped nanobat-like CuO nanostructures by simple, low temperature and cost effective hydrothermal method. Field emission scanning electron microscopy illustrated that these CuO nanostructures have diameter of ∼70 nm, thickness of ∼8 nm and length of ∼174 nm. Structural analysis reveals that the CuO nanostructures have a high crystal quality with monoclinic crystal structure. X-ray photoelectron spectroscopy studies demonstrate that the sample is composed of CuO. The Raman study also indicates the single phase property and high crystallinity of as-grown CuO nanostructures. The plausible growth mechanism for the formation of nanobat-like CuO structure is proposed.     

Photochemical synthesis of copper nanoparticles incorporated in poly(vinyl pyrrolidone)

The effect of the presence of poly(vinyl pyrrolidone) (PVP) on the copper nanoparticle formation, obtained by UV irradiation of ethanol solution of Cu(acac)₂ (acac = 2,4-pentanedionato), was investigated. At 254 nm, in conditions of light completely absorbed by complex, the PVP exhibited protective and stabilizing effects, as shown by the formation of a colloidal copper solution and by a block of the heterogeneous process, which leads to thin film formation on the quartz walls. The colloidal solution was tested for several months by plasmon position and it was found that it remained unaltered in inert atmosphere, but returned to the starting complex on contact with air. The PVP ability to control the particle size was investigated by carrying out photoreduction sensitized by Hacac at 254 and 300 nm, in the presence of PVP concentration varying from 0 to 0.2 M. In this range it was possible to obtain copper nanoparticles of dimensions decreasing from 30 to 4 nm. Besides this, the PVP (0.005–0.05 M) role as sensitizer was investigated by irradiating solutions of Cu(acac)₂ at 300 nm which is an inactive wavelength for copper reduction by direct light absorption. It was found that the PVP was an efficient sensitizer of the copper photoreduction. The nanoparticles were characterized by plasmon band, Trasmission Electron Microscope (TEM) as well as Dynamic Light Scattering (DSL) analysis. The overall results evidence the advantages of the PVP use in the nanoparticle copper formation through the photochemical technique such as the exclusive formation of colloidal copper, their size control, stable colloidal solution and complete return to the starting complex.     

Syntheses of BaCO3 nanostructures by ultrasonic method

BaCO₃ nanostructures were synthesized by the reaction of Ba(CH₃COO)₂ and sodium hydroxide or tetramethylammonium hydroxide (TMAH) by a sonochemical method. Reaction conditions, such as the concentration of the Ba²⁺ ion, aging time and power of the ultrasonic device played important roles in the size, morphology and growth process of the final products. The BaCO₃ nanostructures were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), and the Infrared spectroscopy (IR).     

Magnetic and field emission properties of straw-like CuO nanostructures

This paper reports CuO straw-like nanostructures (nanostraws) synthesized on copper foil substrate through a simple solution method at room-temperature without using any template. The microstructure and morphological of CuO nanostraws were investigated by the X-ray diffraction (XRD) and field emission scanning electron microscope (FESEM), revealing that the straw-like nanostructures were exhibited the nanocrystalline nature with monoclinic structure and monodispersed in large quantity. The possible growth mechanism for the formation of CuO nanostraws products was discussed in detail. In addition magnetic properties and field emission properties of as-obtained products were also investigated.     

Two ultrasonic applications for the synthesis of nanostructured copper oxide (II)

In this paper, we present two aspects of the ultrasonic for the synthesis of CuO (II) nanostructures. In the first ultrasound application, we made a copper tip for an ultrasonic probe transducer and used it for electrolysis and ultrasound irradiation processes. This method is named direct sonoelectrochemistry and compares with conventional electrochemistry. CuO (II) nanostructures are obtained after sintering for both direct sonoelectrochemistry method and conventional electrochemistry method. In the second application of ultrasound, the copper nanostructures were generated by the ultrasound ablation method, and then, the heating process was performed for oxidation. The formation of the copper and CuO (II) nanostructures is confirmed by the powder X-ray diffraction (XRD), the field emission electron microscopy (FESEM), and transmission electron microscopy (TEM). The results show that the direct sonoelectrochemistry method generates CuO (II) nanostructures 4.2 times more than conventional electrochemistry. The crystallite size in the electrochemistry methods and direct sonoelectrochemistry is 28.44 nm and 26.60 nm, respectively. The direct sonoelectrochemistry way is a very flexible method and parameters in electrochemical, ultrasound, and the relationship between them can play an important role in the process of synthesis of nanostructures. The crystallite size in the ultrasound ablation method is 21.13 nm and 25.23 nm for the copper and CuO (II) nanostructures. The most important advantages of this method are green, fast, and high purity of the produced nanostructures.     

Microwave-assistant synthesis of ordered CuO micro-structures on Cu substrate

A mild template-free mixed solution medium with the assistant of microwave method was successfully established to synthesize well-aligned CuO nanostructures. By varying process parameters such as the volume ratio of the mixed solution, different kinds of architectural structures can be controllably synthesized in large quantities. On the basis of the results, it is found that the polarity of the solution plays the key role in controlling the growth of the CuO crystal. The as-prepared CuO products were characterized using diverse techniques including X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The gas sensor property investigation shows that the sensitivities to ethanol of the as-prepared CuO nanostructures are higher than those of normal CuO nanoparticles.     

Microwave-assisted synthesis of flower-like and leaf-like CuO nanostructures via room-temperature ionic liquids

Flower-like and leaf-like cupric oxide (CuO) single-crystal nanostructures have been successfully synthesized using ionic liquid 1-octyl-3-methylimidazolium trifluoroacetate ([Omim]TA) under the microwave-assisted approach. By controlling the concentration of [Omim]TA and reaction temperature, shape transformation of CuO nanostructures could be achieved in a short period of time. The results indicate that ionic liquid [Omim]TA plays an important role in the formation of different morphologies of CuO crystals. The crystal structure and morphology of products were characterized by X-ray powder diffraction (XRD), infrared spectrum (IR), scanning electron microscope (SEM), transmission electron microscopy (TEM), and selected-area electron diffraction (SAED). A possible mechanism for CuO nanostructure was proposed. In addition, UV-vis spectroscopy was employed to estimate the band gap energies of CuO crystals.     

Surface-enhanced absorption by self-organized silver films with aciniform-like nanoaggregates at elevated temperatures

Morphological evolution of silver nanocomposite films prepared by the wet colloidal route and surface-enhanced phenomena on aggregate nanostructures evolved during annealing were investigated. Dramatic changes in morphologies of particles and pores incurred by rearragement, coarsening, premelting, and dewetting of the silver clusters at different concentrations (i.e., mass thicknesses). At a higher mass thickness, the morphological transitions from self-organized nanoaggregates with aciniform pattern at 300 °C to elongated and coarsened particles with circular holes at 400 °C to island clusters at 500 °C occurred in the films. The peculiar absorption with a much redder and broader surface plasmon feature, which gone far beyond the theoretical prediction, induced by the formation of aciniform nanoaggregates embedded in the porous polymer matrix at a critical mass thickness of 9.6 nm during partial degradation of the PVP polymer and rearrangement of silver clusters at 300 °C. The surface-enhanced absorption was dramatically reduced by the elemination of the aggregate nanostructures and the spontaneous formation of the silver nanoisland film at the dewetting temperature of 500 °C.     

CO gas sensing of CuO nanostructures, synthesized by an assisted solvothermal wet chemical route

CuO nanostructures with different morphologies and sizes were grown in a controlled manner using a simple low-temperature hydrothermal technique. By controlling the pH of reaction mixture, spherical nanoparticles and cloudlike CuO structures were synthesized at 100-150 °C with excellent efficiency. These CuO nanostructures have been tested for CO gas monitoring by depositing them as thick films on an interdigitated alumina substrate and evaluated the surface resistance of the deposited layer as a function of operating temperature and CO concentrations. The gas sensitivity tests have demonstrated that the CuO nanostructures, especially cloudlike morphology, exhibit high sensitivity to CO proving their applicability in gas sensors. The role of the nanostructure on the sensing properties of CuO is also discussed.     

In-situ preparation of 1D CuO nanostructures using Cu2(OH)2CO3 nanoribbons as precursor for sacrifice-template via heat-treatment

One-dimensional (1D) CuO nanostructures with nanoribbons, scroll-like structure, arrays of CuO nanoparticles and nanorod-like morphologies respectively, have been successfully prepared using the single-crystalline Cu₂(OH)₂CO₃ nanoribbons as precursors for sacrifice-template via heat-treatments. The series of morphologies images for decomposition kinetics process of Cu₂(OH)₂CO₃ nanoribbons as heat-treatment temperature increased are presented in this work. The result demonstrates that the morphologies of the 1D CuO nanostructures obtained are mainly due to the ribbon-like shape of the precursors. The morphologies of CuO nanostructures also strongly depend on the heat-treatment conditions. At relatively low heat-treatment temperature and heating rate, the morphological features of the precursor can be preserved well, while arrays of CuO nanoparticles can be obtained at higher heating rate and CuO rod-like shape can be prepared with increasing heat-treatment temperature.     

Electrical conductivity studies on PVA/PVP-KOH alkaline solid polymer blend electrolyte

A series of conducting thin-film solid electrolytes based on poly (vinyl alcohol)/ poly (vinyl pyrrolidone) (PVA/PVP) polymer blend was prepared by the solution casting technique. PVA and PVP were mixed in various weight percent ratios and dissolved in 20 ml of distilled water. The samples were analyzed by using impedance spectroscopy in the frequency range between 100 Hz and 1 MHz. The PVA/PVP system with a composition of 80% PVA and 20 wt.% PVP exhibits the highest conductivity of (2.2±1.4) × 10⁻⁷ Scm⁻¹. The highest conducting PVA/PVP blend was then further studied by adding different amounts of potassium hydroxide (KOH) ionic dopant. Water has been used as solvent to prepare PVA/PVP-KOH based alkaline solid polymer blend electrolyte films. The conductivity was enhanced to (1.5 ± 1.1) × 10⁻⁴ Scm⁻¹ when 40 wt.% KOH was added. Paper presented at the International Conference on Functional Materials and Devices 2005, Kuala Lumpur, Malaysia, June 6 – 8, 2005.     

Preparation of size-tunable,highly monodisperse PVP-protected Pt-nanoparticles by seed-mediated growth

We demonstrate a preparative method which produces highly monodisperse Pt-nanoparticles of tunable size without the external addition of seed particles. Hexachloroplatinic acid is dosed slowly to an ethylene glycol solution at 120 °C and reduced in the presence of a stabilizing polymer poly-N-vinylpyrrolidone (PVP). Slow addition of the Pt-salt will first lead to the formation of nuclei (seeds) which then grow further to produce larger particles of any desired size between 3 and 8 nm. The amount of added hexachloroplatinic acid precursor controls the size of the final nanoparticle product. TEM was used to determine size and morphology and to confirm the crystalline nature of the nanoparticles. Good reproducibility of the technique was demonstrated. Above 7 nm, the particle shape and morphology changes suddenly indicating a change in the deposition selectivity of the Pt-precursor from (100) towards (111) crystal faces and breaking up of larger particles into smaller entities.     

静电纺丝纳米ZrO_2:Ti纤维的制备与发光性质的研究

通过静电纺丝和高温煅烧相结合的方法制备了一维钛掺杂氧化锆的纳米纤维。复合纤维在1 000℃煅烧后,由于模板剂、聚乙烯吡咯烷酮(PVP)在高温下的分解,纤维直径大大减小,扫描电镜观察最终得到直径100 nm左右的单斜相纤维。利用稳态光谱和时间分辨光谱技术室温下研究了纤维的光致发光性质。结果表明发射主峰在467 nm的宽带,在350 nm处有一个小肩峰。两种不同的发光行为可以通过ZrO2∶Ti纳米纤维中存在的两种情况的氧空穴作为电子俘获中心来解释。一种由电荷补偿产生的氧空位,俘获电子,产生467 nm处Ti参与的发光现象。另外一种ZrO2表面缺陷导致的氧空穴,对应于350 nm的发光现象,没有发现长余辉现象。测得的激发态寿命短于体材料而长于普通的纳米晶,可能是由于一维纳米结构的独特性质导致的。     

Ultrasound assisted synthesis of {[Cu2(BDC)2(dabco)].2DMF.2H2O} nanostructures in the presence of modulator; new precursor to prepare nano copper oxides

As a new precursor to prepare nano copper oxide, nanostructures of porous metal organic framework (MOF) {[Cu₂(BDC)₂(dabco)].2DMF.2H₂O} (1) have been synthesized in the presence of acetic acid as a modulator via sonochemical method. Different concentrations of metal ion, organic linkers, modulator reagent and also different sonication times were held to improve the quality of nanostructures. Ultrasound irradiation helps nucleation step of the oriented attachment of modulation method and nanoparticles with a few nanorods has been prepared. As prepared MOF was calcinated at 500 °C to prepare nano CuO and Cu₂O. Compound 1, CuO and Cu₂O nanostructures were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray powder diffraction (XRD).     

Syntheses and characterization of Sr(OH)2 and SrCO3 nanostructures by ultrasonic method

The Sr(OH)₂ and SrCO₃ nanostructures were synthesized by reaction of strontium(II) acetate and sodium hydroxide or tetramethylammonium hydroxide (TMAH) via ultrasonic method. Reaction conditions, such as the concentration of the Sr²⁺ ion, aging time, power of the ultrasonic device and alkali salts show important roles in the size, morphology and growth process of the final products. The pure crystalline SrCO₃ were obtained by heating of product at 400 °C. The Sr(OH)₂ and SrCO₃ nanostructures were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), thermal gravimetric (TG), differential thermal analyses (DTA) and the infrared spectroscopy (IR).