Crystallization of CoFeSiB metallic glass induced by long-time ball milling

Milling up to 800 h causes amorphous Co_70.3Fe_4.7Si₁₀B₁₅ alloy, prepared in the form of thin ribbon, to partially crystallize thus forming a powder material consisting of an amorphous phase and fcc-Co nanocrystals with an average grain size of about 10 nm. A gradual increase of the nanocrystalline fcc-Co fraction, produced by ball milling, was detected. Prolonged milling results in destabilization of the fcc-Co phase and oxidation of the powder material (presence of CoO phase after 1500 h of milling). The thermal stability studies of as-quenched and milled Co_70.3Fe_4.7Si₁₀B₁₅ alloy emphasized a two step crystallization behavior. During the first crystallization event, cobalt rich phases, i.e., fcc-Co and hcp-Co crystallize, whereas after the second crystallization event, Co₂B and Co₂Si are formed.     

The structure of amorphous and nanocrystalline W---Fe alloys prepared by high-energy ball milling

Tungsten powder (99.9% purity, 12 μm particle size) was milled in a hardened steel vial with six 440C stainless steel balls for 1–50 h. Because of the hardness of W, contamination and later alloying with Fe from abrasion of the stainless steel balls occurred. X-ray chemical analysis and weight-gain measurements of the milled powder indicated Fe contents varying from 3 at.% after 1 h to approximately 40 at.% after 50h milling. The powder pattern peaks of the nanocrystalline W were subjected to a Fourier analysis to determine the effective particle size and the microstrains within these particles. After 20 h milling, a particle size of 35 Å and microstrains of 0.5% were observed. The diffraction patterns from the W powder milled for 20 and 50 h were also analyzed in terms of the structure factor (interference function) and the atomic distribution function. The 20 h sample was predominantly nanocrystalline with a broad diffuse peak under the (110) and (211) reflections, while the 50 h sample was predominantly amorphous. After subtracting the remnant crystalline peaks, the position of the first peak in the reduced atomic distribution function, G_I(r), was found to be 2.7 Å.     

The effects of annealing temperature on photoluminescence of silicon nanoparticles embedded in SiNx matrix

The effects of the annealing temperature on photoluminescence (PL) of non-stoichiometric silicon nitride (SiN_x) thin films deposited by plasma enhanced chemical vapor deposition (PECVD) using ammonia and silane mixtures at 200 °C were investigated. The optical property and the chemical composition of the films annealed at different temperatures were investigated by PL spectroscopy and Fourier transform infrared absorption spectroscopy (FTIR), respectively. Based on the PL results and the analyses of the bonding configurations of the films, the light emission is attributed to the quantum confinement effect of the carriers inside silicon nanoparticles and radiative defect-related states. These results provide a better understanding of optical properties of silicon nanoparticles embedded in silicon nitride films and are useful for the application of nanosize silicon semiconductor material.     

Facets formation of pyramidal Si nanocrystals selectively grown on Si(0 0 1) windows in ultrathin SiO2 films

We have used in situ scanning tunneling microscopy (STM) to study the facet formation in the selective growth of pyramidal Si nanocrystals on Si(0 0 1) windows in ultrathin 0.3-nm-thick SiO₂ films. Broad (0 0 1) surfaces developed as the top of the crystals, and {1, 1, (2n+1)} (n=1–6) facets formed the sidewalls. As growth continued, the slope angle of sidewall facets increased, and {1, 1, 9} and {1, 1, (2m+1)} (0 <m < 4) facets often came to coexist on the sidewalls. On well-oriented Si(0 0 1) surfaces, layer-by-layer growth in the [0 0 1] direction was dominant. On vicinal Si(0 0 1) surfaces, lateral step growth took place in the initial stage, and the layer-by-layer growth was suppressed until after a large (0 0 1) surface had formed as the top of the crystal.     

Phase diagram of Si nanowire growth by disproportionation of SiO

Silicon nanowires have been grown in a horizontal tube furnace by disproportionation of silicon monoxide in combination with the vapor–liquid–solid mechanism. We present a phase diagram of the nanowire growth, indicating different morphologies for varying growth pressure and temperature. The morphology was characterized by scanning electron microscopy and detailed structural analysis was performed by transmission electron microscopy. A variety of morphologies is found and the optimum parameter range for the growth of straight and uniform nanowires consisting of crystalline silicon cores and amorphous SiO₂ shells is identified and discussed.     

Formation of twinning-superlattice regions by artificial stacking of Si layers

We report about the formation of twinning-superlattice regions in Si epitaxial layers grown by molecular beam epitaxy on Si(1 1 1)()R30°-B surfaces. Twinning-superlattice regions were formed by periodical arrangement of 180° rotation twin boundaries along [1 1 1]-direction and are only separated by a few nanometers. The preparation method consists of repeating several growth, boron-deposition and annealing cycles on boron-predeposited undoped Si substrates. It is shown that the amount of subsurface boron and the growth mode influence the formation of twin boundaries. Only the nucleation of Si on the Si(1 1 1)()R30°-surface covered by at least ML boron results in the formation of 180° rotation twins. The size of superlattice regions is restricted by surface morphology. However, the presented technology should also be suitable to prepare a new type of semiconductor heterostructure based on Si polytypes.     

The effect of the AlxGa1−xN/AIN buffer layer on the properties of GaN/Si(1 1 1) film grown by NH3-MBE

We describe the growth of GaN on Si(1 1 1) substrates with Al_xGa_1−xN/AlN buffer layer by ammonia gas source molecular beam epitaxy (NH₃-GSMBE). The influence of the AlN and Al_xGa_1−xN buffer layer thickness and the Al composition on the crack density of GaN has been investigated. It is found that the optimum thickness is 120 and 250 nm for AlN and Al_xGa_1−xN layers, respectively. The optimum Al composition is between 0.3<x<0.6.     

Large-scale synthesis of ZnSe nanoribbons on zinc substrate

ZnSe nanoribbons have been successfully synthesized on a large scale by solvothermal treatment of Zn and Se powder in the mixture of hydrazine hydrate and diethanolamine at 140 °C for 24 h and subsequent annealing in Ar. The morphology of the final products strongly depended on the volume ratio of hydrazine hydrate and diethanolamine. Scanning electron microscopy (SEM) explorations indicated that the as-prepared ZnSe nanoribbons were mostly about 40 nm in thickness, 100 nm in width, and 50 μm in length. X-ray diffraction pattern (XRD) and transmission electron microscopy (TEM) investigations confirmed that resulting ZnSe nanoribbons are wurtzite structures and have a [0 0 1] growth direction. PL (photoluminescence) spectrum of the products exhibited a visible light emission. Based on these investigations, the products were expected to find wide applications in optoelectronic, field emission and catalytic fields.     

Nonisothermal crystallisation kinetics of amorphous selenium prepared by high-energy ball milling: A comparison with the melt-quenching and thin-film techniques

Differential scanning calorimetry (DSC) studies were performed under nonisothermal conditions at various heating rates for glassy Se made by high-energy ball milling. Comparisons were made between the ball-milling technique and the melt-quenching and thin-film techniques. Well-defined endothermic and exothermic peaks were observed at the glass-transition temperature, T_g, and the onset temperature of crystallisation, T_c. The isoconversional method of Vyazovkin was used to determine the variation in the activation energy for crystallisation with temperature, E_α(T). The value of E_α(T) was dependent on the sample preparation method. The thermal stability of the Se glasses was evaluated by calculation of the temperature difference (T_c ? T_g) and the S-parameter. In addition, the glass-forming ability was estimated by the criteria of reduced glass-transition temperature, T_rg, and the Hruby number, H_R. The structures of the Se samples that resulted from the DSC analysis were identified using an X-ray diffractometer. The glasses formed using the thin film technique were the most stable.     

Magnetic response of Cu (25 wt.%)-316 grade stainless steel processed by ball milling

Powder blend comprising Cu (25 wt.%) and 316-stainless steel (75 wt.%) has been subjected to ball milling upto 70 h followed by isothermal annealing at the temperature range of 350–750 °C for 1 h to investigate the evolution of microstructure and magnetic properties. The ball milling of the powder blends after 10 h has resulted in partitioning of the austenite stabilizing elements such as Ni from 316-stainless steel to elemental Cu leading to the transformation of the Bravais lattice of the Fe-rich phase from fcc (γ) to bcc (α). During further ball milling of the powder mixture upto 20 h, the α-Fe has dissolved completely in Cu, leading to the formation of partial amorphous phase after 70 h of milling. The amorphous phase of the alloy has been found to stable after annealing at 350 °C and super paramagnetic in nature. Annealing of the alloy at higher temperatures has resulted in precipitation of nanocrystalline bcc-Fe in the Cu evolving ferromagnetic properties. Annealing at 750 °C has resulted in collapse of the hysteresis loop due to the diminished exchange interaction as the result of grain coarsening of the α-Fe and Cu.     

Epitaxial growth of ZnO thin films on Si substrates by PLD technique

Epitaxial ZnO thin films have been grown on Si(1 1 1) substrates at temperatures between 550 and 700 °C with an oxygen pressure of 60 Pa by pulsed laser deposition (PLD). A ZnO thin film deposited at 500 °C in no-oxygen ambient was used as a buffer layer for the ZnO growth. In situ reflection high-energy electron diffraction (RHEED) observations show that ZnO thin films directly deposited on Si are of a polycrystalline structure, and the crystallinity is deteriorated with an increase of substrate temperature as reflected by the evolution of RHEED patterns from the mixture of spots and rings to single rings. In contrast, the ZnO films grown on a homo-buffer layer exhibit aligned spotty patterns indicating an epitaxial growth. Among the ZnO thin films with a buffer layer, the film grown at 650 °C shows the best structural quality and the strongest ultraviolet (UV) emission with a full-width at half-maximum (FWHM) of 86 meV. It is found that the ZnO film with a buffer layer has better crystallinity than the film without the buffer layer at the same substrate temperature, while the film without the buffer layer shows a more intense UV emission. Possible reasons and preventive methods are suggested to obtain highly optical quality films.     

Green synthesis by diethylene glycol based solution process and characterization of SnS nanoparticles

Uniform near‐spherical SnS nanoparticles were prepared by a hydrazine hydrate‐assisted diethylene glycol solution synthesis based on the reaction of tin dichloride (SnCl₂·2H₂O) with thioacetamide (H₃CCSNH₂). The as‐prepared SnS nanoparticles were characterized by XRD, FETEM, EDS, XPS and UV‐vis‐NIR spectrophotometer. The results showed that the SnS nanoparticles had orthorhombic crystal structure, good stoichiometry and indirect bandgap of ∼1.1 eV. The nanoparticle size could be controlled by changing injection temperature. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Sol-gel synthesis and characterization of adsorbent and photoluminescent nanocomposites of starch and silica

Using sol-gel method, mesoporous and photoluminescent silica nanocomposites of soluble starch have been synthesized and characterized. Different ratios of H₂O, TEOS and EtOH were used at fixed template (soluble starch) and catalyst (NH₄OH) concentrations to obtain materials of different performances in terms of heavy metal binding from a solution which has been monitored using Cd(II) as representative divalent heavy metal ion. Optimum material was obtained when H₂O, TEOS and EtOH were used in 14:1:2 ratio. This sample was not only an efficient metal ion adsorbent but also had an intense luminescence in ultra-violet region and potentially may be used in silicon-based UV-emitting devices. Metal binding by the material was further enhanced after calcination (at 800 °C in air) while its luminescence had a multipeak profile in UV-visible region. In a batch adsorption study, calcined hybrid composite (0.25 g/L) could remove 98.5% Cd(II) from 100 mg/L Cd(II) solution in 2 h. The chemical, structural and textural characteristics of the synthesized materials have been investigated using Fourier Transform Infrared Spectroscopy (FTIR), X-rays Diffraction (XRD), Thermal Analysis (TGA/DTA), Photoluminescence (PL), Brunauer-Emmett-Teller Analysis (BET) and Scanning Electron Microscopy (SEM).     

The synthesis and structural characterization of silyl-substituted fluorenes

Three silyl-substituted fluorenes have been prepared by direct synthetic methods and structurally characterized by X-ray diffraction. The three silyl-substituted fluorenes studied were 9-trimethylsilylfluorene (1), 9-(tert-butyldimethyl)silylfluorene (2), and 2,7-di-tert-butyl-9-trimethylsilylfluorene (3). Complex 1 is orthorhombic, P2₁2₁2₁, a = 6.2681(14) Å, b = 14.329(3) Å, c = 15.231(4) Å, Z = 4. Complex 2 is monoclinic, P2₁/c, a = 12.1953(10) Å, b = 6.9977(6) Å, c = 19.6536(17) Å, = 93.818(2), Z = 4. Complex 3 is monoclinic, P2₁/c, a = 11.9954(9) Å, b = 9.8978(7) Å, c = 18.5464(13) Å, = 92.456(2), Z = 4. The long carbon–silicon bonds effectively remove any significant intramolecular interactions as little distortion is exhibited around the sp ³-carbon atom and the fluorenyl backbone demonstrates near planarity. The bulky silicon substituents also prevent intermolecular interactions, as only a few close contacts less than 4.0 Å exist in all three solid state structures.     

Structure and properties of nanocomposites prepared from ball milled 6061aluminium alloy with ZrO2 nanoparticles

Ball milling of 6061 aluminum alloy and nanocrystalline ZrO₂ powder allowed to obtain homogeneous mixture of nanocrystalline aluminum solid solution of grain size near 50 nm and ZrO₂ particles. The ZrO₂ particles are partially transformed after milling from tetragonal to the monoclinic crystal structure. After hot pressing in vacuum at temperature of 380 °C bulk nanocomposites were obtained of porosity below 1% consisting of aluminum solid solution of the average grain size near 80 nm and nano‐size ZrO₂ particles. Partial recrystallization occurred after hot pressing particularly near particles boundaries, where elongated recrystallized grains free from ZrO₂ nanoparticles of thickness near 1 μm and length of a few μm were identified. Estimated fraction of recrystallized grains was below 10%. The compression strength approaching 1000 MPa was obtained in composites containing 20% ZrO₂ nanoparticles, what is more than reported for ultra and nano‐grain 6XXX aluminum alloys. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Rapid synthesis of copper nanoparticles by sodium hypophosphite reduction in ethylene glycol under microwave irradiation

This paper presents a rapid method for preparation of copper metal nanoparticles by reducing CuSO₄·5H₂O with NaH₂PO₂·H₂O in ethylene glycol under microwave irradiation. The influences of the reaction parameters, such as the concentrations of reducing agent and protective polymer time of microwave irradiation, on the size and agglomeration of copper nanoparticles were investigated by X-ray powder diffraction and transmission electron microscope. Well-dispersed copper nanoparticles with diameter of about 10 nm were obtained. The use of microwave irradiation accelerated the reaction rate and benefited the dispersion and the particle size distribution of the nanoparticles.     

Facile synthesis of monodisperse MnO nanoparticles from bulk MnO

A simple method is presented for the one-pot synthesis of monodisperse MnO nanoparticles (NPs) using bulk MnO as the starting material. In the proposed approach, bulk MnO powder is dissolved in hot oleic acid to form manganese oleate (Mn(RCOO)₂) and a decomposition process is then performed to obtain MnO NPs. The proposed method is environmentally friendly in that the only by-product is water, which can be easily distilled out. Conceptually, the synthesis method can be viewed as a controlled dissolution recrystallization process. It is shown that the size of the NPs can be controlled over the range of 6–32 nm via an appropriate specification of the precursor-to-oleic acid ratio and the reaction temperature (by the choice of an appropriate high b.p organic solvent). Finally, the size-dependent magnetic properties of three different monodisperse MnO NPs (7.7 nm, 19.4 nm and 31.7 nm) are studied. It is shown that the monodisperse MnO NPs exhibit a weak ferromagnetic behavior due to uncompensated surface spins at low temperatures.     

Hydrothermal synthesis and luminescent properties of YBO3:Tb3+ uniform ultrafine phosphor

The pure hexagonal phase YBO₃:Tb³⁺ phosphors with good crystallinity and uniform size were prepared by hydrothermal reaction (HR). The particle size and morphology can be well controlled by adjusting the concentration of ammonium acetate and varying the reaction temperature and time. The phosphor prepared by HR emits an intense green light at 543 nm, which is stronger than that from crystals synthesized by solid-state reaction (SR). The influence of Tb³⁺-doping concentration on the crystallization and luminescent properties were investigated. The results showed that the samples exhibited a higher quenching concentration of Tb³⁺ in comparison with those prepared by the SR. The phenomena were also discussed.     

Hydrothermal synthesis of mesostructured aluminosilicate nanoparticles assisted by binary surfactants and finely controlled assembly process

Mesostructured aluminosilicate nanoparticles with narrow grain size distribution have been hydrothermally prepared for the first time with assistance of binary surfactants and separate hydrolysis and assembly of inorganic precursors. Compared to the sample assembled at room temperature, condensation degree and aluminum stability were greatly improved using hydrothermal treatment. The formation of nanoparticles consists of two steps, that is, the hydrolysis of silica precursor via catalysis by an acidic aluminum salt, followed by facile assembly into mesostructured nanocomposites with cationic micelles by addition of condensation catalyst. Simultaneously, nonionic polyethylene glycol (PEG-4000) present in this process would surround the formed nanoparticles through hydrogen-bonding interactions, thereby tailoring the grain size distribution and preventing aggregation and growth of inter-nanoparticles during the hydrothermal treatment process. The microstructure and chemical compositions of these products were thoroughly characterized by XRD, SEM, TEM, N₂ sorption and ²⁷Al MAS NMR techniques.     

Facile and one-pot synthesis of magnetic nanoparticles containing mesoporous carbon

Abstract

Magnetic nanoparticles containing mesoporous carbon materials have been synthesized via an one-pot strategy associated with a direct carbonization process from resol, metal ion sources (Co(NO₃)₂·6H₂O, Ni(NO₃)₂·6H₂O) and triblock copolymer F127. The samples exhibited well-ordered 2-dimensional (2-D) hexagonal mesostructures with p6mm symmetry. The Brunauer-Emmet-Teller (BET) surface area and pore size 1.0wt%Co- and 1.0wt%Ni-FDU-15(700) with 1.0?wt% Co and 1.0?wt% Ni content were 700, 528 m²/g and 17.2, 36.4 Å, respectively, after carbonization at 700?°C. The saturation magnetization values of 1.0wt%Co- and 1.0wt%Ni-FDU-15(700) after carbonization at 700?°C were 1.3 and 1.0?emu/g, respectively.