Hydroxylapatite nanoparticles obtained by fiber laser-induced fracture

This work presents the results of laser-induced fragmentation of hydroxylapatite microparticles in water dissolution. Calcined fish bones in form of powder, which were previously milled to achieve microsized particles, were used as precursor material. Two different laser sources were employed to reduce the size of the suspended particles: a pulsed Nd:YAG laser and a Ytterbium doped fiber laser working in continuous wave mode. The morphology as well as the composition of the obtained particles was characterized by scanning electron microscopy (SEM), energy dispersive X-ray (EDX) spectroscopy and conventional and high resolution transmission electron microscopy (TEM, HRTEM). The results show that nanometric particles of hydroxylapatite and β-tricalcium phosphate as small as 10 nm diameter can be obtained.     

Laser-assisted production of tricalcium phosphate nanoparticles from biological and synthetic hydroxyapatite in aqueous medium

Pulsed laser ablation technique has attracted great attention as a method for preparing nanoparticles. In this work, calcined fish bones and synthetic hydroxyapatite, have been used as target to be ablated in de-ionized water with a pulsed CO₂ laser to produce calcium phosphate nanoparticles. The obtained nanoparticles were amorphous and spherical in shape with a mean diameter of about 25 nm. The microanalyses revealed that nanoparticles obtained from the synthetic HA undergo transformation to tricalcium phosphate. While nanoparticles obtained from the biological hydroxyapatite mostly preserve the composition of precursor material.     

Third-order nonlinear optical properties of silver nanoparticles mediated by chitosan

Silver nanoparticles in chitosan medium were prepared by the chemical reduction method. Silver nitrate and hydrazine were used as the precursor and reducing agent in the present of chitosan as a natural host polymer. The samples are characterized by UV–visible spectroscopy, X-ray diffraction (XRD) and transmission electron microscopy (TEM). The measurements of nonlinear optical properties were defined by Z-scan technique using green CW laser beam operated at 532 nm wavelengths. Thermal effect has a dominant role in the overall material nonlinearity with CW laser. It is shown that the synthesized samples have a negative nonlinear refractive index.     

Characteristics of ultrafine tungsten particles produced by Nd:YAG laser irradiation

Ultrafine particles of tungsten were synthesized by the synchronized irradiation of a substrate in low He gas pressure with two pulsed Nd:YAG lasers. The primary particles have diameters of several nm as measured by transmission electron microscopy (TEM). An agglomeration of the primary particles was generated under high pressure and high laser power conditions. An electron diffraction analysis of the particles indicates that there exist two types of material structure: crystalline and amorphous-like. The size distribution was measured by a low-pressure differential mobility analyzer (LP-DMA). The peak of the size distribution was shifted from several nm to the tens of nm level with increasing pressure.     

Multiporous ceria nanoparticles prepared by spray pyrolysis

The morphology of ceria nanoparticles prepared by spray pyrolysis (SP) from cerium (III) acetate and cerium (III) nitrate hydrate precursors were characterized by transmission electron microscopy. It was observed that using the nitrate as a precursor, particles containing multiple pores in the core can be prepared preferentially as opposed to the acetate precursor, when particles with predominantly a single pore were obtained. It was also found that the number of pores in the particles strongly correlates with the particle diameter. It is shown that predominantly multiporous particles for possible catalytic applications may be obtained by selecting particles with diameters between 50 and 100 nm and using cerium nitrate hydrate as a precursor. A mechanism leading to formation of multiporous ceria nanoparticles in the case of using the nitrate precursor in the SP process is discussed based on thermogravimetric analysis (TGA) data.     

CdSe/ZnSe核-壳结构纳米粒子合成新方法

报道用“一步”合成新方法制备了CdSe/ZnSe核-壳结构的发光纳米粒子.该方法是将锌的前驱体注入表面Se富集的CdSe发光纳米粒子溶液中,通过Zn²⁺与Se共价键结合,从而在CdSe发光纳米粒子的表面形成ZnSe壳.分别通过X射线粉末衍射、光电子能谱、透射电镜、紫外-可见吸收光谱和光致发光光谱,对核-壳结构的发光纳米粒子的结构及光学性质进行了表征.结果表明,以较宽带隙的ZnSe在较窄带隙的CdSe纳米粒子表面形成的壳层有效地钝化了CdSe纳米粒子的表面缺陷,明显地提高了室温下CdSe纳米粒子的光致发光效率.X射线粉末衍射表明随着Zn²⁺的不断注入,CdSe/ZnSe的衍射峰逐渐移向ZnSe衍射峰.光电子能谱数据显示,Zn2p的双峰分别位于1020,1040eV附近,通过与体材料ZnO相比,确定为Zn²⁺的光电子发射,说明Zn是以共价键形式存在于CdSe纳米粒子的表面.透射电镜照片显示纳米粒子具有良好的单分散性,核-壳结构的发光纳米粒子直径较CdSe核的直径明显增加.     

Structural, optical and electrical characterization of antimony-substituted tin oxide nanoparticles

Antimony-doped tin oxide (ATO) nanostructures were prepared using chemical precipitation technique starting from SnCl₂, SbCl₃ as precursor compounds. The antimony composition was varied from 5 to 20 wt%. The lower resistance was observed at composition of Sn:95 and Sb:05, when compared with undoped and higher doping concentration of antimony. The average crystalline size of undoped and doped tin oxide was calculated from the X-ray diffraction (XRD) pattern and found to be in the range of 30-11 nm and it was further confirmed from the transmission electron microscopy (TEM) studies. The scanning electron microscopy (SEM) analysis showed that the nanoparticles agglomerates forming spherical-shaped particles of few hundreds nanometers. The samples were further analyzed by energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and electrical resistance measurements.     

Sphere-shaped SiGe micro/nanostructures with tunable Ge composition and size formed by laser irradiation

SiGe spheres with different diameters are successfully fabricated on a virtual SiGe template using a laser irradiation method. The results from scanning electron microscopy and micro-Raman spectroscopy reveal that the diameter and Ge composition of the SiGe spheres can be well controlled by adjusting the laser energy density. In addition, the transmission electron microscopy results show that Ge composition inside the Si Ge spheres is almost uniform in a well-defined, nearly spherical outline. As a convenient method to prepare sphere-shaped SiGe micro/nanostructures with tunable Ge composition and size, this technique is expected to be useful for Si Ge-based material growth and micro/optoelectronic device fabrication.     

Laser-driven synthesis and magnetic properties of iron nanoparticles

Nanoparticles of iron have been prepared by laser-driven decomposition of iron pentacarbonyl vapor. In this method, an infrared laser rapidly heats a dilute mixture of precursor vapors to decompose the precursor and initiate particle nucleation. It was found that when using SF₆ as a photosensitizer during the synthesis, ferrous fluoride (FeF₂) was produced as an undesired byproduct in the product powder. The particle size, composition, and crystalline structure have been characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and X-ray photoelectron spectroscopy (XPS). Results of magnetization measurements for small iron nanoparticles (about 5 nm diameter) are also presented, showing superparamagnetic behavior at room temperature, and a blocking temperature near 125 K.     

Synthesis of Nanoscale Bimetallic Particles in Polyelectrolyte Membrane Matrix for Reductive Transformation of Halogenated Organic Compounds

Nanosized Fe/Ni and Fe/Pd particles were synthesized in the polyacrylic acid (PAA)/polyether sulfone (PES) composite membrane matrix for reductive transformation of halogenated organic compounds (HOCs). The advantages of using membrane to immobilize nanoparticles are the reduction of particles loss, prevention of particles agglomeration, and potential application of convective flow. Cross-linked PAA/PES composite membranes containing metal ions as particles precursor were prepared by heat treatment with ethylene glycol (EG) as a cross-linking agent. Nanoscale metal particles were formed and immobilized inside the membrane matrix after reduction with sodium borohydride. Membrane morphology and structure were observed by scanning electron microscopy (SEM). Particle size and distribution were characterized by SEM and transmission electron microscopy (TEM). Energy dispersive X-ray spectroscopy (EDS) was used to obtain the qualitative and quantitative element information of particles. A specimen-drift-free EDS line profile and EDS mapping system was performed in a scanning transmission electron microscopy (STEM) to determine the two-dimensional element distribution of iron and nickel in the nano domain. In the dechlorination study with trichloroethylene (TCE) as a representative HOCs, rapid and complete destruction of TCE was achieved by using nanosized bimetallic Fe/Ni or Fe/Pd in PAA/PES composite membranes. Typically more than 95% of 10 mg/l TCE was reduced within 1 h. Ethane was found in the headspace as the main product.     

Preparation and characterization of polyvinyl alcohol—chitosan biocompatible magnetic microparticles

This work addresses the obtaining of biocompatible magnetic polyvinyl alcohol—chitosan microspheres, specifically tailored/functionalised to bind directly blood toxins using an emulsion crosslinking preparation method. The following synthesis parameters were studied: water to oil phase ratio, polyvinyl alcohol molecular weight, chitosan to polyvinyl alcohol weight ratio, surfactant composition and concentration of the crosslinking agent. These parameters were optimized for producing a high yield of colloidally stable and uniformly sized particles with significant magnetization of saturation, bearing surface amino groups that can be further used to bind blood toxins directly. The particles were characterized regarding their size distribution and surface charge (laser diffraction analysis), morphology (transmission electron microscopy), magnetic properties, chemical composition (Fourier transform infrared spectroscopy) and concentration of the surface amino groups (conductometric titration).     

A novel route to aligned nanotubes and nanofibres using laser-patterned catalytic substrates

We describe the generation of aligned carbon nanotube bundles and films by pyrolysis of solid organic precursors (for example 2-amino-4,6-dichloro-s-triazine, s-triaminotriazine) at 950-1050 °C over laser-patterned thin metal (Fe, Co, Ni) films, deposited on silica substrates. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) studies reveal that surface roughness of the laser-etched catalytic substrates plays a key role in achieving control of nanotube growth. We believe that, during the etching process, the energised (ablated) metal clusters condense and recrystallise evenly, possibly as the metal oxide, within the edges or surface of the eroded regions. During pyrolysis these catalytic particles, embedded in the silica substrates, are responsible for carbon agglomeration and subsequent tube axial growth, suggesting that nanotube alignment strongly depends upon the etching conditions (for example laser power, pulse duration, and focal distance). The pyrolysed products (usually nanotubes or nanofibres) were characterised by SEM, high-resolution transmission electron microscopy (HRTEM), electron energy loss spectroscopy (EELS) and energy dispersive X-ray spectroscopy (EDX). Samples containing only small amounts of amorphous carbon and other carbonaceous particles are notably absent. We observe that the degree of graphitisation is dependent upon the catalyst and the organic precursor. Interestingly, a nitrogen content З% was detected within the nanofibres, which exhibit corrugated graphite-like morphologies. This pyrolytic method may be used to advantage in generating aligned heteroatomic nanostructures such as B_xC_yN_z systems.     

In situ monitoring of laser cleaning by coupling a pulsed laser beam with a scanning electron microscope

Lasers have proved to be effective tools for material processing at the micron and nanometer scales. In particular, laser interaction with nanostructures offers the unique advantage of highly localized excitation and heating. In this study, a short-pulsed laser beam is coupled to a scanning electron microscope, without disturbing the microscopy function, in order to study in situ laser cleaning of individual submicron particles from a silicon substrate. The substrate conditions before and after particle removal were inspected by electron microscopy. The mechanisms of particle removal and the underlying dynamic coupling of the laser radiation associated with particle cleaning are investigated. PACS 42.62.Cf; 42.82.Gw; 81.65.Cf; 07.78.+s     

New aspects on pulsed laser deposition of aligned carbon nanotubes

We have grown carbon nanotubes (CNT) by pulsed laser deposition (PLD) at 1000 °C in Ar atmosphere. A Nd/YAG laser was used for irradiation of a graphite target containing Ni and Co rods. High-resolution scanning electron microscopy (HRSEM) and transmission electron microscopy (TEM) images showed that “closed” carbon nanotubes were grown between clusters of metallic particles, so that the individual nanotubes were arranged in parallel to each other forming a shape of “Rope-Bridge”. The nanotubes structure was analyzed by high-resolution transmission electron microscopy (HRTEM) and their type was found to be of MWNT, containing about five SWNT. Total diameter was 5-20 nm and their length was about 1 μm. High homogeneous distribution carbon nanotubes were grown and different structures were observed such as well-aligned carbon nanotubes, bamboo-like and Y-junction carbon nanotubes.     

Characterization of scraps produced by the industrial laser cutting of steels

We have studied some properties relevant for technological applications of the debris produced by industrial laser cutting of steels. The investigated material is made up of spheroidal particles, hollow and solid, which get oxidized over the cutting process, and that we have reduced afterwards in a H₂ atmosphere. The samples, before and after the reduction, were characterized by X-ray diffraction, scanning electron microscopy, specific surface area and Mössbauer spectroscopy. We have found that, after the reduction treatment, the shape remains unchanged but that the chemical composition and the physical properties of the external and internal surface structures are modified. In particular, the specific surface area of the material increased by one order of magnitude.     

Following the evolution of morphology, composition and crystallography of alumina based catalysts after laser ablation: Implications for analysis by LA-ICP-AES

Fundamental understanding of aerosol formation during laser ablation is important for the development of LA-ICP analysis of complex samples. Using a Lina Spark Atomizer™, the application of this technique to the field of heterogeneous catalysis gave an accuracy of 5–15% while extreme values of +100% could be obtained in some cases. To improve understanding of laser ablation processes, particles generated during ablation of alumina based catalysts were collected and analysed using different microscopy and surface analysis techniques. Morphological study by scanning electron microscopy showed that most of the particles leaving the ablation cell were nanoparticle aggregates generated from vapor condensation. An XRD study of these aerosols revealed that the condensation converge on the formation of a spinel structure with large coherence domains. Elemental composition of the aerosol was also followed and exhibited differences between a catalyst containing large Mo concentration or low Pt concentration.     

The effects of hydrogen plasma pretreatment on the formation of vertically aligned carbon nanotubes

The effects of H₂ plasma pretreatment on the growth of vertically aligned carbon nanotubes (CNTs) by varying the flow rate of the precursor gas mixture during microwave plasma chemical vapor deposition (MPCVD) have been investigated in this study. Gas mixture of H₂ and CH₄ with a ratio of 9:1 was used as the precursor for synthesizing CNTs on Ni-coated TiN/Si(1 0 0) substrates. The structure and composition of Ni catalyst nanoparticles were investigated by using scanning electron microscopy (SEM) and cross-sectional transmission electron microscopy (XTEM). Results indicated that, by manipulating the morphology and density of the Ni catalyst nanoparticles via changing the flow rate of the precursor gas mixture, the vertically aligned CNTs could be effectively controlled. The Raman results also indicated that the intensity ratio of the G and D bands (I_D/I_G) is decreased with increasing gas flow rate. TEM results suggest H₂ plasma pretreatment can effectively reduce the amorphous carbon and carbonaceous particles and, thus, is playing a crucial role in modifying the obtained CNTs structures.     

Determination of particle size in multiphase blends by different methods

Different methods for characterizing the morphology of multiphase blends were applied to a blend of thermoplastic polyurethane with 20 wt% polypropylene as the dispersed phase. Optical microscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), and light scattering were compared. The microscopy methods were evaluated with respect to their suitability for quantitative image analysis for determination of the particle size distribution. Comparison of the particle size distributions revealed that the dependence of the measured particle size on the method of preparation and technique was not very pronounced. The main difference resulted from cutting the particles outside their maximum diameter. The measured particle sizes determined with methods that analyze the whole particles, such as SEM on separated particles and laser light scattering, are larger than those measured on cut specimens. The factor 4/π valid in monodisperse systems for the ratio between the real particle size and that measured on sections was found also to be applicable to this polydisperse blend system. Although light micros-copy requires the least preparation efforts, it is a reliable method for this blend system.     

Synthesis,characterization and mechanical properties of nylon–silver composite nanofibers prepared by electrospinning

Silver (Ag) nanoparticles (∼3 nm) were synthesized using silver nitrate as the starting precursor, ethylene glycol as solvent and poly (N-vinylpyrrolidone) (PVP) introduced as a capping agent. These nano-Ag particles were reinforced in nylon matrix by electrospinning of nylon-6/Ag solution in 2,2,2-trifluoroethanol and composite nanofibrous membranes were synthesized. The effects of solution concentration and relative humidity (RH) on the resultant fibrous membranes were studied. Scanning electron microscopy and Transmission electron microscopy was used to study the size and morphology of the fibers. It was observed that concentration and RH could be used to modulate the fiber diameter. Tensile test was used to evaluate the mechanical property of these electrospun composite membranes. The composite membranes showed higher strength (approx. 2–3 times increase in strength) compare to as synthesized nylon fibers.     

物理分析技术在无机氧化物晶体结构表征中的应用

以氯化锌和氢氧化钠为主要原料,采用简单液相法,通过改变反应液的组成,制备出了针状、棒状、片状和花状四种不同形貌的ZnO微/纳米晶体。应用X-射线粉末衍射仪（XRD）,扫描电子显微镜（SEM）、高分辨透射电子显微镜（HRTEM）及选区电子衍射仪（SEAD）对产物进行表征,获得了ZnO物相、形貌与微观结构的重要信息。