Surfactant-Mediated Synthesis of Functional Metal Oxide Nanostructures Via Microwave Irradiation-Assisted Chemical Synthesis

In the present work we report a rapid microwave irradiation-assisted chemical synthesis technique for the growth of nanoparticles, nanorods, and nanotubes of a variety of metal oxides in the presence of an appropriate surfactant (cationic, anionic, non ionic and polymeric), without the use of any templates. The method is simple, inexpensive, and helps one to prepare nanostructures in quick time, measured in seconds and minutes. This method has been applied successfully to synthesize nanostructures of a variety of binary and ternary metal oxides such as ZnO, CdO, Fe2O3, CuO, Ga2O3, Gd2O3, ZnFe2O4, etc. There is an observed variation in the morphology of the nanostructures with changes in different process parameters, such as microwave power, irradiation time, identity of solvent, type of surfactant, and its concentration.

Aging response and its effect on the functional properties of Cu–Al–Ni shape memory alloys

The β-phase aging response of Cu–Al–Ni single crystal shape memory alloys (SMAs) within the temperature range of 473–573 K has been investigated. Alloys in austenitic (Cu–14.1Al–4Ni wt.%, alloy A) and martensitic (Cu–13.4Al–4Ni wt.%, alloy M) conditions at room temperature were considered. Aged samples show presence of β1′ and γ1′ martensites in both the alloys and formation of γ2 precipitates in the alloy A. The differential scanning calorimetry (DSC) thermograms of the aged samples show increase in transformation temperatures as well as transformation hysteresis with aging. Dynamic mechanical analysis (DMA) was conducted on both the alloys to ascertain the role of precipitates and martensitic transition on tan δ, which characterizes the damping behaviour of the material. With aging, a steady decrease in tan δ value was observed in both the alloys, which was attributed to the decrease in the number of interfaces per unit area with increasing aging temperature. Moreover, in alloy A, as the volume fraction of precipitate increases with aging, the movement of martensitic interfaces is restricted causing a decreased tan δ.

Investigation of dye functional group on the photocatalytic degradation of dyes by nano-TiO2

The photocatalytic degradation of five anionic, eight cationic and three solvent dyes using combustion-synthesized nano-TiO2 (CSTiO2) and commercial Degussa P-25 TiO2 (DP-25) were evaluated to determine the effect of the functional group in the dye. The degradation of the dyes was quantified using the initial rate of decolorization and mineralization. The decolorization of the anionic dyes with CSTiO2 followed the order: indigo carmine > eosin Y > amido black 10B > alizarin cyanine green > orange G. The decolorization of the cationic dyes with DP-25 followed the order: malachite green > pyronin Y > rhodamine 6G > azure B > nile blue sulfate > auramine O approximate to acriflavine P approximate to safranin O. CSTiO2 showed higher rates of decolorization and mineralization for all the anionic dyes compared to DP-25, while DP-25 was better in terms of decolorization for most of the cationic dyes. The solvent dyes exhibited adsorption dependent decolorization. The order of decolorization and mineralization of the anionic and cationic dyes (a) with CS TiO2 and DP-25 was different and correlated with the surface properties of these catalysts (b) were rationalized with the molecular structure of the dye and the degradation pathway of the dye. (C) 2009 Elsevier B.V. All rights reserved.

Nanoscale Heterostructures with Molecular-Scale Single-Crystal Metal Wires

Creating nanoscale heterostructures with molecular-scale (<2 nm) metal wires is critical for many applications and remains a challenge. Here, we report the first time synthesis of nanoscale heterostructures with single-crystal molecular-scale Au nanowires attached to different nanostructure substrates. Our method involves the formation of Au nanoparticle seeds by the reduction of rocksalt AuCl nanocubes heterogeneously nucleated on the Substrates and subsequent nanowire growth by oriented attachment of Au nanoparticles from the Solution phase. Nanoscale heterostructures fabricated by such site-specific nucleation and growth are attractive for many applications including nanoelectronic device wiring, catalysis, and sensing.

Advanced transmission electron microscope triboprobe with automated closed-loop nanopositioning

Here the design and operation of a novel transmission electron microscope (TEM) triboprobe instrument with real-time vision control for advanced in situ electron microscopy is demonstrated. The NanoLAB triboprobe incorporates a new high stiffness coarse slider design for increased stability and positioning performance. This is linked with an advanced software control system which introduces both new and flexible in situ experimental functional testing modes, plus an automated vision control feedback system. This advancement in instrumentation design unlocks new possibilities of performing a range of new dynamical nanoscale materials tests, including novel friction and fatigue experiments inside the electron microscope.

Surface diffusion driven nanoshell formation by controlled sintering of mesoporous nanoparticle aggregates

We report a general method for the synthesis of hollow structures of a variety of functional inorganics by partial sintering of mesoporous nanocrystal aggregates. The formation of a thin shell initiates the transport of mass from the interior leading to growth of the shell. The principles are general and the hollow structures thus produced are attractive for many applications including catalysis, drug delivery and biosensing.

Functional nanoporous structures by partial sintering of nanorod assemblies

We present a general method for the synthesis of functional nanoporous structures by heat treating a loose compact of nanorods. Partial sintering of such a compact leads to spherodization of the nanorods and their fusion at the contact regions leading to an interconnected porous microstructure. The pore diameter can be controlled by changing the original nanorod diameter. We illustrate the generality of the method using TiO2, ZnO and hydroxyapatite as model systems; the method is applicable for any material that can be grown in the form of nanorods. The kinetics of the sintering process can be significantly enhanced in systems in which additional driving forces for mass transport arise from phase transitions proving an ultrafast pathway for producing biphasic porous structures. The possibility of producing hierarchical porous structures using fugitive sintering aids makes this process ideal for a variety of applications including catalysis, photoanodes for solar cells and scaffolds for biomedical applications.

Superconductivity in rapidly quenched metallic systems with nanoscale structure

Nanocomposites of Al?In, Al?Pb, and Zn?Pb have been prepared and characterized using rapid quenching techniques and the nature of superconducting transitions in them has been studied by resistivity measurements. The precipitated second phases (In and Pb) have particle sizes (d) of a few tens of nanometers such that ?0?d?dmin, where ?0 is the superconducting zero temperature coherence length and dmin is the minimum particle size that supports superconductivity. The onset of superconductivity generally starts in samples with d??0 and progressively other grains with d??0 become superconducting. We suggest that the proximity effect of the matrix plays a significant role. In an Al?In system, even with 40?wt.% In, the zero resistivity state is obtained at T?1.33 times the Tc of Al. But in Al?Pb and Zn?Pb, the zero resistivity state is obtained at T?4 and 5 times the Tc of Al and Zn with only 10�15 wt?% Pb, respectively.

Porous, catalytically active palladium nanostructures by tuning nanoparticle interactions in an organic medium

We present a simple template-free method for the synthesis of interconnected hierarchical porous palladium nanostructures by controlling the aggregation of nanoparticles in organic media. The interaction between the nanoparticles is tuned by varying the dielectric constant of the medium consistent with DLVO calculations. The reaction products range from discrete nanoparticles to compact porous clusters with large specific surface areas. The nanoclusters exhibit hierarchical porosity and are found to exhibit excellent activity towards the reduction of 4-nitrophenol into 4-aminophenol and hydrogen oxidation. The method opens up possibilities for synthesizing porous clusters of other functional inorganics in organic media.

Nanoscale ZnO/CdS heterostructures with engineered interfaces for high photocatalytic activity under solar radiation

Semiconductor based nanoscale heterostructures are promising candidates for photocatalytic and photovoltaic applications with the sensitization of a wide bandgap semiconductor with a narrow bandgap material being the most viable strategy to maximize the utilization of the solar spectrum. Here, we present a simple wet chemical route to obtain nanoscale heterostructures of ZnO/CdS without using any molecular linker. Our method involves the nucleation of a Cd-precursor on ZnO nanorods with a subsequent sulfidation step leading to the formation of the ZnO/CdS nanoscale heterostructures. Excellent control over the loading of CdS and the microstructure is realized by merely changing the initial concentration of the sulfiding agent. We show that the heterostructures with the lowest CdS loading exhibit an exceptionally high activity for the degradation of methylene blue (MB) under solar irradiation conditions; microstructural and surface analysis reveals that the higher activity in this case is related to the dispersion of the CdS nanoparticles on the ZnO nanorod surface and to the higher concentration of surface hydroxyl species. Detailed analysis of the mechanism of formation of the nanoscale heterostructures reveals that it is possible to obtain deterministic control over the nature of the interfaces. Our synthesis method is general and applicable for other heterostructures where the interfaces need to be engineered for optimal properties. In particular, the absence of any molecular linker at the interface makes our method appealing for photovoltaic applications where faster rates of electron transfer at the heterojunctions are highly desirable.

Nanoscale Ag–Pd and Cu–Pd alloys

Nanoparticles of Ag-Pd and Gu-Pd alloys with diameters in the 5-40 nm range have been prepared over the entire range of compositions, by employing the heterogeneous reaction of dry methanol or ethanol with intimate mixtures of AgNO3+PdOx and CuOx+PdOx, respectively. The nanoscale alloys have been characterized by energy-dispersive Xray (EDX) analysis, transmission electron microscopy (TEM) and X-ray diffraction (XRD). All the alloy particles possess the fee structure and can be obtained in bulk quantities.

ChemInform Abstract: Chemical Design of Solid Inorganic Materials

Newer strategies for the synthesis of inorganic solids have made a great impact on present-day materials chemistry. In this article, typical case studies of synthesis involving new methods and soft chemical routes are discussed besides recent results from nebulized spray pyrolysis and synthesis of nanoscale metal and alloy particles.

Synthesis and properties of nanodispersed granular materials

Nanometric granular materials represent a new class of materials with significant promise. We shall discuss in this paper two phase granular materials where one of the phases having nanometric dimension is embedded in a matrix of larger dimension. These materials show many interesting properties which include structural, magnetic and transport properties, The phase transformation of the embedded particles shows distinctive behavior and yields new insight. We shall first highlight the strategy of synthesis of these materials through rapid solidification. This will be followed by three examples where the nanoscale dimension of the embedded particles play a unique role. These are melting and solidification of the nanodispersed embedded particles and the superconducting transition. (C) 1997 Elsevier Science S.A.

Nanoscale embedded alloy particles through rapid solidification: the case of Al-Pb-In and Cu-Fe-Si

Rapid solidification techniques can be used to produce the embedded nanoparticles in a desired matrix. The origin and morphology of these small particles and their transformation behaviour are still not fully understood. In this paper, we discuss the issues involved and present some interesting results in Al-Pb-In and Cu-Fe-Si systems.

The melting and solidification of nanoscale Bi particles embedded in a glassy and crystalline matrix

We report the formation of an amorphous phase in nanosized Pi particles embedded in an Al-based glassy alloy matrix. High-resolution electron microscopy (HREM) has been used to show that the particles contain crystalline and amorphous portions. A depression of the melting point by more than 100 K of the crystalline portion of the Pi particles was found by differential scanning calorimetric studies and by in-situ electron microscopy using a heating stage. The same techniques established the absence of an amorphous phase in the particles when the matrix is crystallized. It is shown that the formation of the amorphous phase and the depression of the melting point cannot be explained by the pressure developed by the volume change during solidification in this constrained system.