An attempt to reduce the effect of major toxic components namely phosphine ligands and unsaturated solvents as being used in conventional nanocrystal synthesis, has been made with a new binary ligand, and a reusable solvent N-octadecane for a smokeless and clean synthesis procedure. The optimized effects of the two ligands oleic acid and octadecyl amine on the nucleation rate and growth of CdSe nanocrystals (NCs) are reported and substantiated by AFM analysis. Oleic acid accelerates particle ripening and nuclei growth, but inhibits nucleation whereas octadecyl amine catalyses nucleation and very gradually improves growth to obtain small stable NCs. Another important feature of the present study is the replacement of 1-octadecene by a competitive N-octadecane as a solvent in such ligand mediated nanocrystal synthesis. The GCMS analysis reports a recovery of 95% of solvent after reuse, thus opening a scope for environmental friendly processes.

Doping of a heteroatom such as nitrogen in carbon nanomaterials provides a means to tailor their electronic properties and chemical reactivities. In this article, we present simple methods to synthesize carbon quantum dots (CQDs) with high nitrogen doping content (18–22%), involving the reaction of glucose in the presence of urea under hydrothermal conditions or by microwave irradiation. The N-doped carbon quantum dots (N-CQDs) show high aqueous solubility and tunable photoluminescence (PL). Interaction of N-CQDs with exfoliated graphene or dimethylaniline quenches PL. Interaction of N-doped as well as undoped C-dots with electron-donating tetrathiafulvalene and electron-withdrawing tetracyanoethylene has been examined. The intense blue PL of CQDs has been exploited to produce white light by mixing the CQDs with yellow light emitting ZnO nanoparticles or graphene oxide. The N-doped CQDs exhibit superior photocatalytic activity compared to pristine CQDs.

A facile and reproducible low-temperature (80 °C) solution route has been introduced to synthesize ZnO ellipsoids on silicon substrate without any pretreatment of the substrate or organic/inorganic additives. Scanning electron microscopy, transmission electron microscopy, and x-ray diffraction spectroscopy are performed to analyze the structural evolution, the single crystalline nature, and growth orientation at different stages of the synthetic process. The sequential formation mechanisms of heterogeneous nucleation in primary and secondary crystal growth behaviors have been discussed in detail. The presented results reveal that the morphology of micro/nanostructures with desired features can be optimized. The optical properties of grown structures at different stages were investigated using cathodoluminescence (CL). The monochromatic CL images were recorded to examine the UV and visible band emission contributions from the different positions of the intermediate and final structures of the individual ZnO ellipsoid. Significant enhancement in the defect level emission intensity at the central position of the structure reveals that the quality of the material improves as the reaction time is extended.

The thermoelectric properties of Bi2Sr2Co2Ox (BSC-222) bulk materials prepared by three different processing methods, i.e., conventional sintering, hot pressing, or partial melting, were investigated and compared. The electrical current, temperature difference for Seebeck coefficient, and thermal diffusion were measured in the same direction. The hot pressing and partial melting are effective processing methods for improving the electrical transport property in BSC-222 bulk materials due to an improvement of density in hot-pressed samples or by grain growth during partial melting process. For partially melted samples, a decrease in the thermal conductivity is also observed. The highest dimensionless thermoelectric figure of merit (ZT) values have been obtained in the sample prepared by partial melting method, for which ZT has been increased by a factor of 2.7 by comparison with bulk materials prepared by conventional sintering. At 700 °C in air, ZT value reaches 0.27 for partially melted Bi2Sr2Co2Ox bulk materials. This study shows that optimized electrical and thermal transport properties can be achieved in BSC-222 bulk materials possessing microstructures with both large average grain size and appropriate bulk density.

In this article, a comprehensive investigation on the thermal properties of Yb3Al5O12 is conducted, including Debye temperature, thermal expansion coefficient (TEC), thermal diffusivity, heat capacity, and thermal conductivity. The calculated Debye temperature of Yb3Al5O12 from the measured elastic properties is 625 K. The linear and volumetric thermal expansions of Yb3Al5O12 from 298 to 1273 K are (7.83 ± 0.14) × 10−6 and (23.74 ± 0.42) × 10−6 K−1, respectively. The linear TEC of the polycrystalline bulk Yb3Al5O12 determined by dilatometer is (8.22 ± 0.3) × 10−6 K−1. The measured thermal conductivities of Yb3Al5O12 are 4.67 and 2.05 W (m K)−1, respectively, at 300 and 1400 K. The estimated minimum thermal conductivity, κmin, is 1.22 W (m K)−1. The high temperature thermal conductivity is close to the evaluated κmin, which is lower than most commonly used thermal barrier coating (TBC) material such as Y2O3-stabilized-ZrO2 (YSZ). The unique combination of these properties renders Yb3Al5O12 being a very promising candidate material for TBC.

The solid-state reaction of yttrium aluminum garnet (YAG, Y3Al5O12) during the heat treatment of Y2O3 and Al2O3 powder mixtures, differing in particle size and size ratio, was quantified using in situ high-temperature x-ray analysis and Rietveld refinement. Y2O3 particle size has the most profound effect on YAG formation. When the Y2O3 particle size was decreased from 5000 to 30 nm (on reaction with 270 nm Al2O3), the YAG formation rate increased from 20 to 48 vol% min−1 over the temperature range of 1350–1450 °C. In this case, the final YAG content increased from 75 to 91 vol%. A simple model that includes the reactant particle coordination number, and thus particle size ratio, shows that when the size ratio (dA/dY) is >1 diffusion through the alumina powder is rate controlling whereas when the ratio is <1, diffusion through the yttria, intermediate phases, and YAG is rate controlling.

CuInS2 thin films with thickness ranging from 196 to 1000 nm were prepared from a source containing CuInS2 nanocrystals by using thermal evaporation method. Annealed films of CuInS2 show the quasi-amorphous to crystalline phase transition, probed through x-ray diffraction (XRD), UV-visible spectrometer, and Raman spectroscopy. From XRD, the tetragonal distortion (η) is found to be ≈1, confirming the arrangement of an extended double lattice structure of chalcopyrite phase. The surface morphology of quasi-amorphous film exhibits a very smooth surface, whereas crystalline film shows a very rough surface of CuInS2 as observed from atomic force microscopy. Crystallite size and rms roughness increase from 23 to 310 nm and from 1.5 to 36.5, respectively, with increasing film thickness as well as with increasing annealing temperature due to the crystallization process. Micro-Raman study evidencing the presence of a strong Raman A1 mode at 303 cm−1, due to the symmetric vibration of anion sublattice of CuInS2 structure. A fundamental band edge is observed in as-deposited quasi-amorphous CuInS2 films, while bulk energy band absorption and excitonic band transition are observed in crystalline films. A sharp drop in both reflectance and transmittance near the energy band gap region is observed in thick films due to a very strong absorption of crystalline phase of CuInS2.

Nanoparticles of ∼55 nm in diameter have been found to significantly increase the fracture toughness of nanocomposites with a ductile polymer matrix. This paper presents a comparative study of the effectiveness of micrometer-sized and nanosized elastomeric particles in improving the fracture toughness and strength of polymeric adhesives. Particular focuses are on the effects of particle size, matrix ductility, and adhesive thickness on the shear strength and fracture toughness. The results reveal that for an epoxy adhesive cured with a J400 hardener, nanosized particles can produce nearly 18 times more increase in fracture toughness than what can be achieved using micrometer-sized particles at the same volume fraction of 5.0 vol%. This huge improvement of adhesives' fracture toughness by nanosized particles is similar to that observed in bulk nanocomposites, indicating that the superior toughening mechanism of nanosized elastomeric particles is equally effective in thin adhesives constrained by stiff adherends.

Nb, F-codoped TiO2 (NFT) nanoparticles are prepared via hydrothermal processes using Nb2O5 and hydrofluoric acid as doping source. Nb and F distribute homogeneously in the NFT nanoparticles as shown in scanning transmission electron microscopy elemental mappings. The codoping of Nb and F improves the crystallinity of TiO2 significantly and increases the Ti3+ concentration, which results in the enhancement of electron injection and in the increase of the charge-transfer ability in dye-sensitized solar cells. The relative energy conversion efficiency can be 66.1% higher than that of the cell, based on pure TiO2, when the Nb:F:Ti molar ratio is about 0.03:0.15:0.97.

Magnetron-sputtered Ni(W) films appear to possess a high density of nanotwins oriented parallel to the film surface which highly influences the properties of Ni(W) films. A sophisticated analysis method for describing the stacking sequence of close-packed atomic layers by statistical parameters has been developed which is based on the evaluation of intensity streaks in reciprocal space measured by (x-ray) synchrotron diffraction. In particular, the degree of hexagonality introduced by twinning into these ideally face-centered cubic-stacked films can be quantified. The validity of the proposed analysis has been confirmed by direct observation of the stacking sequences of close-packed layers using (high-resolution) transmission electron microscopy. It has been shown that the degree of hexagonality in the as-deposited state is practically proportional to the W content. Further, the thermal stability of the nanotwins increases with increasing W content which can be understood by the appearance of hexagonal close-packed-like domains exhibiting an intrinsic thermodynamic stability.

We have studied the magnetoresistance (MR) of hydrogen plasma-treated pure ZnO wires of tens of micrometer diameter at different temperatures. A negative MR of 1% at 8 T applied field is measured for all wires at 4 K, independent of the temperature (300 K … 773 K) used during the hydrogen treatment. However, a positive MR develops, the higher the treatment temperature. The MR can be explained with a semiempirical model taking into account local magnetic moments and the s–d exchange interaction. These results together with field anisotropy in the MR indicate the appearance of magnetic order due to the hydrogen treatment in agreement with recently published reports on the influence of hydrogen in bulk ZnO single crystals. Hydrogen doping may provide a way to trigger defect-induced magnetism in small oxide structures.

Plasmonic Ag nanoparticles (AgNPs) with narrow distribution were successfully loaded on graphitic carbon nitride (g-C3N4) sheet by thermal polymerization of melamine precursor and a simple wet-chemical pathway in the presence of polyvinylpyrrolidone (PVP). N,N-dimethylformamide (DMF) was used as an efficient reducing agent as well as a solvent and its presence facilitated homogeneous distribution of AgNPs under mild reaction condition and easy control of its particle growth under different precursor amounts. Ag/g-C3N4 composites of different Ag content were prepared, and the phase, chemical structure, morphologies, electronic and optical properties of Ag/g-C3N4 heterostructures were well characterized, respectively. The photocatalytic activity of Ag/g-C3N4 composites was evaluated by the decolorization of methyl orange (MO), and they exhibited superior photocatalytic activity to bulk g-C3N4 under visible-light irradiation. Influence of Ag content to photocatalytic activity was also discussed and possible mechanism was explored based on the analysis of photoluminescence spectra (PL) and photodecoloration activity.

This paper aims to develop an integrated method to extract elastic–plastic parameters from a single instrumented spherical indentation curve. The expression of unloading work is chosen to be combined with the previous work [P. Jiang, T.H. Zhang et al, J. Mater. Res.24(3), 1045 (2009)]. An extensive numerical study was performed to examine the effectiveness of the method. Refitting Jiang's similarity solution based on the numerical study was also performed to simplify the form of the expression and improve the accuracy of the elastic–plastic parameters extracted. The results show that the error of our solution was less than ±5%. We also examined its sensitivity by assessing levels of artificial error introduced into the testing parameters used in the method. These results show that this method can provide reasonable estimates of the elastic–plastic parameters for most common metals.

Field emission (FE) measurements are reported from carbon nanotube (CNT) fibers and laser-patterned free standing films fabricated by direct online condensation from a floating catalyst chemical vapor deposition reactor. Fiber and film cathodes showed stable emission in the 1–2 mA current (I) range at maximum cathode temperatures less than 1000 °C; film cathodes show localized heating at the triangular tips and higher maximum temperatures than the fibers. Fowler–Nordheim (FN) analysis indicated a change in the morphology of the emitters with increasing external electrical field (Eext). Fiber cathode I–Eext data are interpreted as FN emission from the fiber tip which is eventually limited by space-charge effects. At higher Eext, FN emission from the fiber sidewall occurs. The single fiber cathode stopped emitting abruptly when field induced self-heating effects became significant. For CNT films, self-heating effects can destroy a portion of the film, but FE can still occur from other areas.

This study demonstrates a highly sensitive humidity sensor based on treated multiwalled carbon nanotube (tr-MWCNT) and hydroxyethyl cellulose (HEC) composite films. Tr-MWCNTs are obtained by mixed acid treatment to enhance their hydrophilicity and improve their dispersion in distilled water. Compared to tr-MWCNT/silicone rubber (SR) composite film, the humidity sensitivity of tr-MWCNT/HEC film is much higher than tr-MWCNT/SR film with the same film thickness. The humidity sensing mechanisms of tr-MWCNT/HEC composites are explained by electron donation model and swelling mechanism. Speaking and blowing experiments were also carried out and the results show that tr-MWCNT/HEC composite film is sensitive to both speaking and blowing; furthermore, it can distinguish the small humidity level difference between speaking and blowing. Other sensing characteristics, including response and recovery time, stability, and temperature effect, are also investigated. The high humidity sensitivity of tr-MWCNT/HEC composite film indicates that it can be an excellent humidity sensitive material.

The aim of this research study is to produce high-quality TiO2 nanotube arrays using porous alumina templates. The templates are fabricated through anodizing bulk aluminum foils which can be utilized for the production of thick alumina templates. To produce the nanotube arrays, the alumina template pores are filled with the precursor sol by applying a DC electric field. Then, the deposited nanotubes are heat treated at 320 °C for 2 h and, subsequently, sintered for 2 h at 400 and 750 °C to obtain nanotubes with pure anatase and rutile phases, respectively, as confirmed by x-ray diffraction data. Scanning and transmission electron microscopy (SEM and TEM) investigations show that the nanotubes have been deposited in the channels of the nanoporous alumina template. Also, SEM investigations show the existence of a vast area of TiO2 nanotube arrays when we use semiconductor alumina templates.

The solid-state phase transitions of bismuth(III) oxide (Bi2O3) nanoparticles were investigated by complementary methods such as differential scanning calorimetry, differential thermal analysis with combined thermogravimetry and mass spectrometry, and high-temperature x-ray diffraction as compacted nanopowder. At room temperature the particles resided in the β-phase, which is usually a metastable high-temperature phase of bulk Bi2O3. The complementary experimental methods were linked and a nanophase (tetragonal β-phase) → bulk-phase (monoclinic α-phase) transition was identified which was preceded by crystal growth and evaporation of O and C containing species. It was also shown that the atmosphere (more precisely its absolute pressure) has an influence on the transition behavior. An interpretation was proposed that successfully explains all observations from this work and from literature: A sudden destabilization takes place around 735 K due to the loss of the stabilizing, carbonized surface. This leads to the observed transformation to the bulk-phase. But if the particles are smaller than a certain, critical size in the nanorange and are not allowed to grow, they remain in the nanophase until they melt.

In situ transmission electron microscopy (TEM) analysis shows that submicrometer grains formed by ultrasonic impact treatment (UIT) of sensitized 5456-H116 Al–Mg alloy products are thermally stable up to ∼300 °C which is consistent with previous research on annealing of heavily deformed Al–Mg. Grain growth occurs above 300 °C with significant growth at ∼400 °C. Grain growth continued upon heating to 450 °C; the grain size did not significantly increase when the temperature was held at 450 °C long term. In situ TEM revealed a duplex microstructure that was not fully recrystallized. The activation energy for grain growth was determined to be ∼32 kJ/mol. The submicrometer grains produced by UIT offer improved resistance to fatigue and corrosion. The majority of sensitized 5456-H116 failures are sensitive to the material's surface properties and operational service temperature; the stability of the submicrometer grains in the UIT Al–Mg makes them more stable in practical operations where increase in the material temperature is an issue.

Ceramic wafers of alumina (Al2O3) were produced by tape casting of aqueous slurry followed by vacuum sintering. The binder system used to form the tape casting slurry is a copolymer of isobutylene and maleic anhydride, which is environmentally friendly, marketed under the name ISOBAM. The rheological properties of the slurries were studied by varying solid loading and binder addition level. Through the optimization of plasticizer addition, green tapes were casted with excellent plasticity and a thickness of 240–740 μm. The tapes displayed a post-sintering thickness of 150–660 μm. The morphologies, as well as the fracture surface and the as-sintered surface of the powder were examined using a scanning electron microscope (SEM). The in-line transmittance of the transparent unpolished Al2O3 wafers with a thickness of 660 μm was found to be 72% at a wave length of 5 μm and 26% at a wave length of 600 nm.

Adsorbents with high specific surface areas, developed porosities, and sustainable CO2 capture capacity (∼180 mg/g at 25 °C, 1 bar) were prepared by KOH activation of hydrothermally carbonized carboxymethylcellulose (CMC). Condensed aromatic carbon materials (CSc) with particle diameters of 2–3 μm and many oxygen-containing groups on their surfaces can be obtained after hydrothermal treatment of CMC; these materials are similar to glucose-derived hydrothermal carbons. The activation conditions, including activation ratio and activation temperature, significantly influence the structure and morphology of the adsorbents. In turn, the pore structures, specific surface areas, and adsorption conditions significantly affect the adsorption capacities of these new adsorbents. For samples with the same activation ratio, those with higher specific surface areas show higher CO2 capture capacities at 25 °C and 1 bar. Under these conditions, for samples with different activation ratios, the capacity is dominated by the microporosity development and, in particular, the high volume of smaller micropores (d = 0.4–0.9 nm); when the adsorption pressure is decreased to 0.1 bar, the CO2 capture ability becomes closely correlated with the number of ultramicropores (d < 0.7 nm).