Morphological control of Ni/NiO core/shell nanoparticles and production of hollow NiO nanostructures

Chemical synthesis coupled with a microwave irradiation process allowed for the control of size (6–40 nm), shape, and shell thickness of Ni/NiO core/shell nanoparticles. In this unique synthetic route, the size of Ni nanoparticles (NiNPs) was strongly influenced by the nickel salt-to-stabilizer ratio and the amount of the stabilizer. Interestingly, it was observed that the shape of the nanoparticles was altered by varying the reaction time, where longer reaction times resulted in annealing effects and rupture of the stabilizer micelle leading to distinct shapes of Ni/NiO core/shell nanostructures. Product cooling rate was another important parameter identified in this study that not only affected the shape, but also the crystal structure of the core/shell nanoparticles. In addition, a simple and cost-effective method of microwave irradiation of NiNPs led to the formation of distinctly shaped hollow NiO nanoparticles. These high surface area core/shell nanoparticles with well-controlled morphologies are important and can lead to significant advancement in the design of improved fuel cells, electrochromic display devices, and catalysis systems.     

Synthesis and magnetic properties of carbon-coated Ni/SiO_2 core/shell nanocomposites

A simple method for the synthesis of carbon-coated Ni/SiO2 core/shell nanocomposites is reported. The Ni nanoparticles were coated with silica layers via a combined procedure of sol-gel fabrication and hydrogen reduction prior to carbon coating via acetylene decomposition at an appropriate temperature. It was found that the anti-acid ability of the Ni/SiO2 composites was greatly enhanced after carbon coating. The results of magnetization measurement show that the real part (μ′) of complex permeability of the as-obtained sample is almost independent of frequency, and the imaginary part (μ″) stays small up to a frequency of 1 GHz. The encapsulation of Ni particles with SiO2 results in the rise of Ni nanoparticles resistivity. The outcome is the reduction in effect of eddy current at high frequency, making the real part μ′ almost constant and the imaginary part μ″ very small. Thus, this simple method may be effective for preparing composites of soft magnetic properties, especially in the high-frequency range.     

Structural and magnetic properties of polymer-stabilized tetragonal Ni nanoparticles

Ni nanoparticles (Ni-NPs), with diameter (D) ranging 5–30 nm, were synthesized by reducing nickel chloride with NaBH₄ in the presence of polymer molecules of poly-vinyl alcohol (PVA) in cold water. Nickel chloride was dispersed in the PVA molecules which stabilized the resulting Ni-NPs. Experiments were carried out with and without PVA to elucidate the effect of PVA molecules on the structural and magnetic properties of Ni-NPs. It was found that both uncoated (uc) and PVA-coated (pc) Ni-NPs exhibit a tetragonal (t) crystal structure, i.e. different from the cubic (fcc) structure of bulk nickel. pc Ni-NPs (paramagnetic in nature) converted to fcc Ni (spherical shape, D ～ 12 nm) on annealing at 573 K in air, exhibiting a saturation magnetization M _s = 20.5 emu/g, squareness ratio M _r /M _s = 0.48 and coercivity H _c = 248 Oe, which is higher than the bulk Ni (0.7 Oe). uc Ni-NPs showed little improvement in M _s and H _c on air annealing. The core–shell structure resulted in a high H _c value in stable pc Ni-NPs in air. Electron magnetic resonance revealed exchange interaction between the core and shell, which changes on annealing in air.     

Tunning exchange bias in inverted antiferromagnetic/ferromagnetic core/shell nanoparticles by binary alloy shells

A detailed investigation of exchange bias properties of an inverted nanoparticle with an antiferromagnetic core and a ferromagnetic binary alloy shell of the type $B_x{C}_{1?x}$ is presented by benefiting from Monte Carlo simulations. Exchange bias displays a non-monotonic behavior with the varying value of the concentration the type-B magnetic components, x. Coercivity exhibits a monotonic or a non-monotonic variation with x depending on the relative strength between unlike magnetic components in the shell. Particular attention has also been given to determine the effects of the cooling field process on the magnetic properties of the nanoparticle. Numerical results obtained in this work present a different physical mechanism and an alternative way for tuning the exchange bias and coercivity of bimagnetic core/shell nanoparticles.     

Magnetic/non-magnetic nanoparticles films with peculiar properties produced by ultrashort pulsed laser deposition

Films of magnetic nanoparticles uniformly mixed with non-magnetic nanoparticles have been produced by ultrashort pulsed laser deposition. These films present innovative characteristics with respect to their counterparts produced by standard techniques, as for example nanosecond laser ablation or sputtering, due to the peculiar shape and preferential distribution of their constituent nanoparticles. In the present investigation, the difficult coalescence among the deposited nanoparticles, specific characteristic of the ultrashort pulsed laser deposition, is particularly stressed for what concerns its effect on the collective magnetic behaviour. In particular, we observed that, even for a significant fraction of magnetic particles, the films exhibit an unusual high remanent magnetization, together with relatively low values of saturation and coercive fields, showing a strong squareness of the hysteresis loops. In perspective, these nanogranular films appear very promising for potential application as permanent magnets and in magnetic recording.     

Superlattice CoCrPt/Ru/CoFe structure fabricated by pulsed laser deposition

The synthetic antiferromagnets (SAF) have been used in spin-valve sensor in data storage industry [1]. We report a new hard/Ru/soft sandwich structure (SHBL) fabricated by pulsed lased deposition to replace current single layer structure for information recording application. SHBL consists of two magnetic layers separated by thin nonmagnetic layers, typically with Ru layers of 0.7-1.2 nm, through which antiferromagnetic coupling is induced. Varying the relative thickness of the magnetic layers, the spacer layers, and the type of magnetic materials can alter magnetic properties of CoCrPt/Ru/CoFe superlattice. The coercivity H_c and grain size of magnetic layer is also dependent on the laser fluence. High laser fluence results in both small grain size and high H_c. The observed phenomena are related to high quenching and deposition rates during PLD at high fluence, resulting in more pronounced phase segregation.     

Synthesis and magnetic properties of carbon-coated Ni/SiO2 core/shell nanocomposites

A simple method for the synthesis of carbon-coated Ni/SiO₂ core/shell nanocomposites is reported. The Ni nanoparticles were coated with silica layers via a combined procedure of sol-gel fabrication and hydrogen reduction prior to carbon coating via acetylene decomposition at an appropriate temperature. It was found that the anti-acid ability of the Ni/SiO₂ composites was greatly enhanced after carbon coating. The results of magnetization measurement show that the real part (μ′) of complex permeability of the as-obtained sample is almost independent of frequency, and the imaginary part (μ″) stays small up to a frequency of 1 GHz. The encapsulation of Ni particles with SiO₂ results in the rise of Ni nanoparticles resistivity. The outcome is the reduction in effect of eddy current at high frequency, making the real part μ′ almost constant and the imaginary part μ″ very small. Thus, this simple method may be effective for preparing composites of soft magnetic properties, especially in the high-frequency range. Supported by the Jiangsu Postdoctoral Foundation of Jiangsu Province and the Major Project of National Basic Research Program of China (Grant No. 2005CB623605)     

Numerical study of exchange bias in antiferromagnetic/ferromagnetic core/shell nanoparticles with non-magnetic defects

We perform Monte Carlo simulations for an antiferromagnetic/ferromagnetic core/shell nanoparticle with a doubly inverted structure. We investigate the dependence of the exchange bias field and coercivity on the magnetic dilution of the shell-interface and shell part. It is demonstrated that exchange bias and coercivity can exhibit monotonic or non-monotonic behavior depending on the location of the non-magnetic components. Also, temperature dependence of the exchange bias and coercivity of the system are studied for a particular defect concentration value. Our results provide an alternative way for tunning the magnetic properties of doubly inverted nanoparticles.     

Indomethacin nanoparticles directly deposited on the fluidized particulate excipient by pulsed laser deposition

Nanoparticles of indomethacin (IM), a sparingly soluble drug in water, were prepared by pulsed laser deposition with Nd: YAG laser at 1064 nm. Variation of the deposition rate (DR) with various experimental conditions, such as species and pressure of the background gas, and laser fluence, was discussed. We obtained highest DR, 2.7 g/cm²min, under He at 100 Pa with the laser fluence of 25 J/cm². In the deposited solid product, no trace of drug decomposition was observed by HPLC. Deposition of IM nanoparticles was achieved on the fluidized excipient, potato starch particles of 20 m regime. By TEM observation and zeta potential distribution measurement, we confirmed that surface of excipient particles was fully covered by nanoparticles of IM. Thus, the present method enables us a new method of one-step preparation of drug-excipient nanocomposites to eliminate tedious problems associated with nanoparticles handling.     

Superhydrophobicity of polytetrafluoroethylene thin film fabricated by pulsed laser deposition

Superhydrophobic polytetrafluoroethylene (PTFE) thin films were obtained by pulsed laser deposition (PLD) technique carried out with KrF excimer laser (λ = 248 nm) of about 1 J/cm² at a pressure of 1.33 Pa. The samples exhibit high water contact angle of about 170° and the sliding angle smaller than 2°. From studying the surface morphology of the prepared films, it is believed that the nano-scale surface roughness has enhanced the hydrophobic property of the PTFE. The increase of trapping air and reducing liquid-solid contact area due to the rough surface, as suggested by the Cassie-Baxter's model, should be responsible for superhydrophobicity of the PLD prepared films. This study thus provides a convenient one-step method without using wet-process to produce a superhydrophobic surface with good self-cleaning properties.     

Optical extinction for determining the size distribution of gold nanoparticles fabricated by ultra-short pulsed laser ablation

This work presents a method, based on measurements of the optical extinction spectra, to determine the size of spherical gold nanoparticles produced using the femtosecond laser ablation process in deionized water. By using an improved theoretical model that modifies the contribution of the free electrons to the dielectric function introducing a size-dependent term, it is possible to fit the full experimental extinction spectrum considering a certain size distribution. Additionally, in order to obtain complementary measurements of the size distribution, TEM analysis was performed. The results obtained showed that the predominant nanoparticle size distribution ranges from 1 to 11 nm in terms of radii. An optical extinction measurement together with an appropriate theoretical model based on Mie’s theory represents a simple, low-cost, fast and easy method to describe a multimodal size distribution of spherical gold nanoparticles.     

脉冲激光沉积法制备的Ni1-xFexO稀磁半导体的结构和磁性研究

利用脉冲激光沉积方法制备出了具有室温铁磁性的Ni1-1-xFexO(x=0.02,O.05)稀磁半导体.X射线衍射(XRD)结果表明Ni,1-xFexO的品体结构为Nacl结构,并且在Fe含量较高的Ni095Fe0.05O中出现了少量的a-Fe2O3物相.X射线吸收近边结构谱(XANFS)和X射线光电子能谱(XPs)进一步表明了掺杂的Fe原子替代Ni0日格中Ni原子,并且样品中不存在能够诱导室温磁性的第二相.这些研究结果表明Ni1-xFexO的室温铁磁性是本征的.     

Magnetic properties and characterization of CoCrM/TiCr/Si films produced by pulsed laser deposition

A series of nanogranular CoCrM/TiCr thin films have been fabricated by pulsed-laser deposition on Si(1 1 1) substrates at 450–500 °C. The crystal structure and magnetic properties of these films were investigated. The transmission electron microscope images with selected area diffraction and X-ray diffraction showed that the structure of as-prepared films is dependent on laser energy and deposition temperature. It was found that the microstructure of CoCrM/TiCr films consisted of fine dispersive crystal grains, while the preferential c-axis orientation of films deteriorated when the thickness of CoCr-alloy layer increased along with metal doping into the CoCr films. The magnetic properties of CoCrM/TiCr films formed on Si are strongly dependent on the thickness of magnetic layer, grain structure, and grain shape. Enhancement of coercivity and squareness of the laser-deposited film is probably due to the improvement in the magnetocrystalline anisotropy energy and the reduction in the thickness of magnetic layer.     

Nanofabrication of tungsten supertip by electron-beam-induced deposition

Two methods were used to fabricate tungsten supertips by electron-beam-induced deposition using 200 keV electrons. The first method is stationary deposition of self-standing tips. The smallest lateral size is less than 10 nm with a rather low aspect ratio of tip. High aspect ratio (up to 30) can only be obtained at a big lateral size with a saturated root diameter of 60–65 nm. The other method is scan deposition of self-supporting tip, with a root width of 7–10 nm and a sharp apex in size of 3 nm. Using this method a higher aspect ratio (more than 72) can be achieved at a smaller lateral size, which is better to fabricate fine supertips for usage.     

CdSe &; ZnS core/shell nanoparticles generated by laser ablation of microparticles

Laser Ablation of Microparticles (LAM) is a process of nanoparticle formation in which microparticles in a flowing aerosol are continuously ablated by high-power laser pulses. For the first time, we have produced CdSe/ZnS core/shell nanoparticles using a double ablation apparatus, designed to undergo a two-step LAM process. This process can be inverted to produce ZnS/CdSe core/shell nanoparticles. The present work focuses on the range around ∼15 nm radius heterostructures and uses high-resolution transmission electron microscopy (HRTEM) to image core and shells. For smaller particles, core shell structures have been detected with energy dispersive spectroscopy (EDS) 5 nm spot size beam and fast Fourier transform (FFT) spectra. Differences in the ablation behavior were measured between the two IIB–VIA type semiconductors.     

Structural, electrical and mechanical properties of NiO thin films grown by pulsed laser deposition

Nickel oxide (NiO) thin films were prepared by reactive pulsed laser deposition on thermally oxidized Si substrates in 10 Pa oxygen pressure. The substrate temperature during deposition was varied and its influence on the structural, electrical and nanomechanical properties was studied. It was proved that the structural properties were affected by the increase of substrate temperature improving the crystalline structure. Furthermore, a higher substrate temperature resulted in a thicker NiO film, which was attributed to an increased grain size. This effect influenced the electrical properties, too. Resistivity measurements showed that it increased with the increase of substrate temperature. For the first time, the nanomechanical properties of NiO films were studied. The formation and improvement of crystalline structure affected the nanomechanical properties. Nanoindentation testing of NiO thin films revealed an increase of hardness (H) and elastic modulus (E) and a decrease of surface roughness when increasing the substrate temperature.     

Structure and optical properties of ZnO nanowires fabricated by pulsed laser deposition on GaN/Si(111) films with the use of Au and NiO catalysts

The growth of ZnO nanowires on a Si(111) substrate with a GaN buffer layer by pulsed laser deposition at a high argon pressure and with the use of Au and NiO catalysts has been investigated. Application of the low-temperature NiO catalyst makes it possible to reduce the optimal growth temperature from 900°C (in the case of the Au catalyst) to T = 570°C and grow ZnO nanowires 20 nm in diameter, which are highly-oriented in the direction of the c lattice axis and completely free of dislocations.     

Phase transitions in Co nanoclusters grown by pulsed laser deposition

The crystalline structure of Co clusters embedded in an amorphous Al₂O₃ matrix was studied by transmission electron microscopy (TEM) and electron diffraction (TED). In the first stage of the growth a metastable structure (body-centred-cubic) is observed. A face-centred-cubic phase (fcc) is found when the size of the clusters increases ( diameter > 4 nm). The hexagonal-close-packed phase arises in the fcc phase by a succession of stacking faults at the largest sizes. The mechanisms of phase transformation have been determined by using high resolution electron microscopy (HREM). The chemical nature of the clusters, in particular the existence of Co-O bonds, was investigated by using electron energy loss spectroscopy (EELS). Received 03 July 2000 and Received in final form 22 December 2000     

Synthesis and characterization of Ni magnetic nanoparticles in AlMCM41 host

Superparamagnetic nickel nanoparticles were prepared by incorporating nickel ion into AlMCM41 as a nanoreactor and then reduced with sodium borohydride or H₂ gas. Products were characterized by elemental analysis, transmission electron microscopy, X-ray powder diffraction, and magnetic susceptibility. The nickel particle size and blocking temperature depend on the reduction method.     

Effects of deposition temperature on the structural and morphological properties of SnO2 films fabricated by pulsed laser deposition

Tin oxide (SnO₂) thin films were grown on Si (1 0 0) substrates using pulsed laser deposition (PLD) in O₂ gas ambient (10 Pa) and at different substrate temperatures (RT, 150, 300 and 400 °C). The influence of the substrate temperature on the structural and morphological properties of the films was investigated using X-ray diffraction (XRD), atomic force microscopy (AFM) and scanning electron microscopy (SEM). XRD measurements showed that the almost amorphous microstructure transformed into a polycrystalline SnO₂ phase. The film deposited at 400 °C has the best crystalline properties, i.e. optimum growth conditions. However, the film grown at 300 °C has minimum average root mean square (RMS) roughness of 3.1 nm with average grain size of 6.958 nm. The thickness of the thin films determined by the ellipsometer data is also presented and discussed.