A Novel Hydrothermal Synthesis of Single Crystalline PbS Nanorods and Their Characterization

1.IntroductionDuring the past decade,one-dimensional(1D)nanos-tructures,such as nanorods,nanowires,nanobelts andnanotubes,have attracted increasing attentions due totheir novel electrical,optical and magnetic properties,and their potential applications in nanoscale eletronics,photonics and functional materials[1~3].Great effortshave been made to prepare1D semiconductor nanostruc-tures such as Si nanowires[4],ZnO nanorods[5]and GaNnanowires[6].At the same time,chalcogenide nanostruc-tures su…     

Synthesis of CuS and PbS nanocrystals on the basis of PE/NBR polymer/elastomeric composites for their applications

In this research work, we have presented a chemical method to elaborate the PbS, CuS nanocrystals embedded in a polymer composites matrix. We have used polyethylene and nitrile butadiene rubber PE/NBR as a support for synthesis of lead sulfide (PbS) and copper sulfide (CuS) nanocrystals. The size control and morphology of these (PbS and CuS) nanoparticles have been applied by the method of “layer by layer”. The obtained nanoparticles were characterized by X-ray diffraction (XRD), UV–Vis and Atomic Force Microscopy (AFM). UV–Vis spectroscopy was used to determine simple optical responses, getting the biggest transmittances of CuS and PbS nanoparticles. Measured size of CuS nanoparticles is approximately 5.5–90 nm in different dose. X-ray diffraction (XRD) study confirmed the formation of cubic phase of PbS nanocrystals into the composite matrix. The size of PbS was estimated ∼9 nm. The surface morphology and crystallite sizes were determined by Atomic Force Microscopy measurements.     

Template-free hydrothermal synthesis of PbS nanorod by the oriented attachment mechanism

In this work, PbS nanocubes and nanorods were fabricated via a facile hydrothermal method without using any template and surfactant. The structure and morphology of as-prepared PbS nanocrystals were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and high-resolution transmission electron microscopy (HRTEM). It was found that the anisotropic structure of PbS nanorods were composed of numerous assembled nanocubes, which had an uniform morphology with the mean diameters of about 100-200 nm and lengths of 0.5-7 μm. Furthermore, a possible growth mechanism was proposed to explain the formation of the nanorods on the basis of the time-dependent experimental results.     

Polymer assisted preferential growth of PbS and PbS:Mn nanorods: structural and optical properties

We report here the structural and optical properties of PbS and PbS:Mn nanorods (diameter 30–80 nm) grown in a polymer (polypyrrole) matrix. X-ray diffraction data of nanorods clearly reveals preferential growth of PbS nanorods with a strong lattice distortion from a bulk cubic to tetragonal one. The strain introduced lattice distortion is inherent to the growth process and strongly depends on polymer concentration. The polymer concentration is found to play an important role in controlling the structural properties. The effect of Mn²⁺ incorporation into PbS lattice shows no appreciable change in the structural properties. Optical absorption behaviors in such PbS and PbS:Mn nanorods are also reported. The absorption peak energy shows blue-shift with increase in Mn²⁺ concentration to some critical value beyond which red-shift is observed.     

Synthesis of PbS/poly (vinyl-pyrrolidone) nanocomposite

A simple solution growth method for synthesis of nanocomposite of PbS nanoparticles in poly(vinyl-pyrrolidone) (PVP) polymer is described. The nanocomposite is prepared from methanolic solution of lead acetate (PbAc), thiourea (TU) and PVP at room temperature (∼27 °C). Optical absorption spectrum of PbS/PVP nanocomposite solution shows strong absorption from 300 to 650 nm with significant bands at 400 and 590 nm which is characteristic of nanoscale PbS. Spin-coated nanocomposite films on glass have an absorption edge at ∼650 nm with band gap of 2.55 eV. Fourier transform infrared (FTIR) spectroscopy of PbS/PVP nanocomposite and PVP shows strong chemical bond between PbS nanoparticles and host PVP polymer. The transmission electron microscope (TEM) images reveal that 5-10 nm PbS particles are evenly embedded in PVP polymer. The formation of PbS is confirmed by selective area electron diffraction (SAED) of a typical nanoparticle.     

Fabrication of PbS nanoparticle coated amorphous carbon nanotubes: Structural, thermal and field emission properties

A simple chemical route for the synthesis of PbS nanoparticle coated amorphous carbon nanotubes (aCNTs) was described. The nanocomposite was prepared from an aqueous suspension of acid functionalized aCNTs, lead acetate (PbAc), and thiourea (TU) at room temperature. The phase formation and composition of the samples were characterized by X-ray diffraction and energy dispersive analysis of X-ray studies. The Fourier transformed infrared spectra analysis revealed the attachment of PbS nanoparticles on the acid functionalized aCNT surfaces. Morphology of the samples was analyzed with a field emission scanning electron microscope. UV-Vis study also confirmed the attachment of PbS nanoparticles on the walls of aCNTs. Thermal gravimetric analysis showed that the PbS coated aCNTs are more thermally stable than functionalized aCNTs. The PbS coated aCNTs showed enhanced field emission properties with a turn-on field 3.34 V μm⁻¹ and the result is comparable to that of pure crystalline CNTs.     

Large scale hydrothermal synthesis of PbS nanorods

PbS nanorods with a diameter of 20-50 nm have been synthesized successfully by surfactant-assisted hydrothermal route. The product was over 90% yield according to the amount of Pb(CH₃CHOO)₂ used. Experiments showed that the concentration of N-cetyl-N,N,N-trimethyl- ammonium bromide (CTAB) and thiourea (Tu), reaction time and sulfur sources played important roles in the formation of the PbS nanorods. A reasonable mechanism for the formation of the PbS nanorods is also discussed.     

Synthesis of crystalline and amorphous germanium nanorods

Crystalline and amorphous germanium nanorods have been synthesized by PVD of germanium powders in flowing Ar/H₂ atmospheres. TEM images show diameters of the nanorods ranging from 20 to 200 nm and length up to 5 μm. Selected area electron diffraction indicates that the crystalline nanorods have tetragonal structure. Their growth process has been considered as VLS mechanism.     

Microwave-assisted synthesis of cobalt oxalate nanorods and their thermal conversion to Co3O4 rods

Cobalt oxalate nanorods have been successfully synthesized by a simple microwave-assisted solution approach using an ionic liquid 1-n-butyl-3-methyl imidazolium tetrafluoroborate. Upon thermal decomposition at 400 °C, cobalt oxalate nanorods could be converted to Co₃O₄ rods consisting of nanoparticles. The products were characterized using X-ray powder diffraction, transmission electron microscopy, thermogravimetric analysis and differential scanning calorimetric analysis.     

Nonlinear optical properties of the PbS nanorods synthesized via surfactant-assisted hydrolysis

PbS nanorods were synthesized by surfactant-assisted homogenous hydrolysis. The products were characterized by UV–vis spectrophotometer, X-ray powder diffraction (XRD) and transmission electron microscope (TEM). PbS nanorods were measured by the Z-scan technique to investigate the third-order nonlinear optical (NLO) properties. The result of the NLO measurements shows that the PbS nanorods have the third-order nonlinear optical properties of both NLO absorption and NLO refraction with self-focusing effects. The nonlinear absorption coefficient and refractive index of the PbS nanorods are 2.16 × 10^− 9 m/W and 3.52 × 10^− 16 m²/W respectively.     

Synthesis and characterization of ultra small PbS nanorods in sucrose ester microemulsion

In the present study, we report for the first time the synthesis of ultra small PbS nanorods in a non-ionic sugar based water-in-oil (w/o) microemulsion system using food grade sucrose ester as surfactant. PbS was formed by mixing lead nitrate and thioacetamide in the water core of the microemulsion system. The as-prepared PbS nanorods were characterized by X-ray diffractometry (XRD), uv–visible absorption spectroscopy (UV–VIS), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The diameter of the PbS nanorods were found to be extremely small, which is in the range of 2.64 nm to 2.91 nm depending on reaction aging time. Spherical PbS nanoparticles were formed after 12 h and PbS nanorods were formed after more than 1 day of reaction aging time.     

Surfactant controlled synthesis of crystalline phosphovanadate nanorods

Phosphovanadate nanorods were obtained in a reaction of vanadium (V) oxide as a precursor and a cationic surfactant, dodecylpyridinium chloride, as structure directing template at pH ∼3 at room temperature. The composition and morphology of the nanorods was established by powder X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), fourier transform infra-red spectroscopy (FTIR), thermogravimetric analysis (TGA), transmission electron microscopy (TEM) and atomic force microscopy (AFM). The obtained nanorods have diameters of 40-60 nm with lengths up to 1 μm. The effect of reaction parameters such as concentration of surfactant and pH of the solution on the growth of nanorods has been investigated. A plausible mechanism involving the coalescence of nanoparticle ‘seeds’ leading to one-dimensional nanorods is also discussed. The same reaction when performed under hydrothermal condition, keeping other reaction parameters unchanged, resulted in the formation of phosphovanadate nanospheres of diameter 10-15 nm.     

Preparation of single-crystal copper ferrite nanorods and nanodisks

This article, for the first time, reports the preparation of single-crystal copper ferrite nanorods and nanodisks. Using amorphous copper ferrite nanoparticles synthesized by reverse micelle as reaction precursor, single-crystal copper ferrite nanorods were synthesized via hydrothermal method in the presence of surfactant polyethylene glycol (PEG), however, copper ferrite nanodisks were prepared through the same procedures except the surfactant PEG. The resulting nanomaterials have been characterized by powder X-ray diffraction (XRD), selected electron area diffraction (SEAD), and transmission electron microscopy (TEM). The bulk composition of the samples was determined by means of X-ray photoelectron spectroscopy (XPS).     

Growth of aligned ZnO nanorods on woven Kevlar® fiber and its performance in woven Kevlar® fiber/polyester composites

ZnO nanorods were grown by a seeding treatment on surface-functionalized woven Kevlar® fiber (WKF), and the decorated WKF was used to prepare composites with polyester resin (PES) via vacuum-assisted resin transfer molding. Fourier transform infrared spectroscopy (FT-IR) confirmed the surface functionalization of the WKF. The characteristic peaks of ZnO observed by FT-IR and X-ray diffraction (XRD) indicated the growth of ZnO nanorods on the surface of the WKF. FT-IR analyses of the composites were consistent with an interaction between the WKF, and ZnO and PES. The intensity of the XRD peak for crystalline ZnO increased with increasing growth of the nanorods. The morphology of the nanorods was studied by scanning electron microscopy. The growth of the nanorods increased with increasing treatment time. Thermogravimetric analysis also supported the growth of nanorods. The presence of ZnO nanorods significantly improved the impact resistance of the WKF/PES composites; the penetration thresholds were also determined. The WKF/ZnO/PES composites had substantially higher tensile strengths and moduli than the ZnO-free composites.     

Synthesis and properties of poly(methyl methacrylate-2-acrylamido-2-methylpropane sulfonic acid)/PbS hybrid composite

The synthesis of a new hybrid composite based on PbS nanoparticles and poly(methyl methacrylate-2-acrylamido-2-methylpropane sulfonic acid) [P(MMA-AMPSA)] copolymer is reported. The chemical synthesis consists in two steps: (i) a surfactant-free emulsion copolymerization between methyl methacrylate and 2-acrylamido-2-methylpropane sulfonic acid and (ii) the generation of PbS particles in the presence of the P(MMA-AMPSA) latex, from the reaction between lead nitrate and thiourea. The composite was studied by scanning electron microscopy (SEM), X-ray diffraction, FTIR spectroscopy, thermogravimetric analysis and differential scanning calorimetry. The microstructure observed using SEM proves that the PbS nanoparticles are well dispersed in the copolymer matrix. The X-ray diffraction measurements demonstrate that the PbS nanoparticles have a cubic rock salt structure. It was also found that the inorganic semiconductor nanoparticles improve the thermal stability of the copolymer matrix.     

Growth of PbS nanopyramidal particulate films for potential applications in quantum-dot photovoltaics and nanoantennas

We report a simple interfacial process called the liquid-liquid interface reaction technique (LLIRT) that leads to the formation of nanosized PbS particulate films with hitherto unreported pyramidal morphology. The resultant PbS films were characterized by transmission electron microscopy (TEM) with selected area electron diffraction (SAED), X-ray diffractometery (XRD), atomic force microscopy (AFM), near field scanning optical microscopy (NSOM) and UV-vis spectroscopy. The pyramidal morphology is speculated to originate from the preferred orientation of the 2 2 0 plane of cubic PbS. Our nanopyramidal PbS particulate films display remarkably sharp excitonic peak centered around 656 nm that accounts for a band gap of 1.8 eV suggesting, in turn, their potential application in QD photovoltaics. Interestingly, the feasibility of such nanopyramids to potentially act as nanoantennas (as revealed by the NSOM) is also suggested.     

Preparation and characterization of CuO nanorods by thermal decomposition of CuC2O4 precursor

Synthesis of copper oxide (CuO) nanorods was achieved by thermal decomposition of the precursor of CuC₂O₄ obtained via chemical reaction between Cu(CH₃COO)₂·H₂O and H₂C₂O₄·2H₂O in the presence of surfactant nonyl phenyl ether (9)/(5) (NP-9/5) and NaCl flux. Transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), selected-area electron diffraction (SAED) and high-resolution TEM (HRTEM) were used to characterize the structure features and chemical compositions of the as-made nanorods. The results showed that the as-prepared nanorods is composed of CuO with diameter of 30-100 nm, and lengths ranging from 1 to 3 μm. The mechanism of formation of CuO nanorods was also discussed.     

Room temperature synthesis of In2S3 micro- and nanorod textured thin films

Thin films of indium sulfide (In₂S₃) micro- and nanorods were successfully prepared by sulfurization of electrodeposited metal indium layers. The films were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM) and UV-vis spectroscopy. From XRD and TEM observations it was concluded that the In₂S₃ nanorods and microrods have ∼50 nm and ∼0.5 μm diameter, respectively. A plausible top-growth mechanism was proposed for the formation of the nanorods in which the hydroxide layer was found to play an important role. The micro- and nanorods showed optical bandgap of ∼2.2 and ∼2.54 eV, respectively. This facile and cost effective method may be extended to fabricate other metal chalcogenide nanostructures on solid substrates.     

Growth of PbTe nanorods controlled by polymerized tellurium anions and metal(II) amides via composite-hydroxide-mediated approach

The pure face-centered-cubic PbTe nanorods have been synthesized by the composite-hydroxide-mediated approach using hydrazine as a reducing agent. The method is based on reaction among reactants in the melts of potassium hydroxide and sodium hydroxide eutectic at 170-220 °C and normal atmosphere without using any organic dispersant or surface-capping agent. Scanning electron microscopy, X-ray diffraction, transmission electron microscopy, and energy dispersive X-ray spectroscopy were used to characterize the structure, morphology and composition of the samples. The diameters of nanorods are almost fixed, while the lengths can be tunable under different growth time and temperatures. The growth mechanism of PbTe nanorods is investigated via UV-vis absorption, demonstrating that polymerized tellurium anions and metal(II) amides in the hydrazine hydroxide melts could control the crystallization and growth process of PbTe nanostructures. The band gap of as-synthesized PbTe nanorods has been calculated based on UV-vis-NIR optical diffuse reflectance spectra data.     

Hydrothermal synthesis,characterization and luminescent properties of GdPO4·H2O:Tb nanorods and nanobundles

In this paper, the Tb³⁺-doped GdPO₄·H₂O nanorods and nanobundles have been synthesized by the hydrothermal method with and without glycine, respectively. The X-ray powder diffraction (XRD), thermogravimetric and differential thermal analysis (TG–DTA), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), energy-dispersive spectra (EDS) and photoluminescence (PL) were employed to characterize the as-obtained products. It was found that the addition of glycine and the pH value have crucial influences on the formation of the resulting morphologies and sizes. The possible formation mechanisms for GdPO₄·H₂O:Tb³⁺ nanorods and nanobundles were put forward. A detailed investigation on the photoluminescence of GdPO₄·H₂O:Tb³⁺ different samples revealed that the luminescent properties of products are strongly correlated with the morphologies, sizes, coordination environment and crystal field symmetry.