Ultrasound irradiation based in-situ synthesis of star-like Tragacanth gum/zinc oxide nanoparticles on cotton fabric

Application of natural biopolymers for green and safe synthesis of zinc oxide nanoparticles on the textiles is a novel and interesting approach. The present study offers the use of natural biopolymer, Tragacanth gum, as the reducing, stabilizing and binding agent for in-situ synthesis of zinc oxide nanoparticles on the cotton fabric. Ultrasonic irradiation leads to clean and easy synthesis of zinc oxide nanoparticles in short-time at low-temperature. FESEM/EDX, XRD, FT-IR spectroscopy, DSC, photocatalytic activities and antimicrobial assay are used to characterize Tragacanth gum/zinc oxide nanoparticles coated cotton fabric. The analysis confirmed synthesis of star-like zinc oxide nanoparticles with hexagonal wurtzite structure on the cotton fabric with the average particle size of 62 nm. The finished cotton fabric showed a good photocatalytic activity on degradation of methylene blue and 100% antimicrobial properties with inhibition zone of 3.3 ± 0.1, 3.1 ± 0.1 and 3.0 ± 0.1 mm against Staphylococcus aureus, Escherichia coli and Candida albicans.     

A new carbon nitride synthesized by shock compression of organic precursors

A series of shock recovery experiments up to ∼50 GPa were carried out on three nitrogen-rich materials of a C–N–O amorphous precursor, dicyandiamide and melamine. The powder X-ray diffractions (XRD) of recovered samples show that carbon nitride phases are formed. They are β-C₃N₄ and a new crystalline phase. The new phase is indexed as a monoclinic cell with a=0.981 nm, b=0.723 nm, c=0.561 nm, β=95.2° and V_cell=0.3966 nm³. Melamine was very stable and did not decompose up to ∼37 GPa. This new phase is considered to form during the adiabatic release process with an extremely high quenching rate (∼10⁹ K/s) and shock compression may provide a novel synthesis route for various C–N phases from appropriate organic materials.     

Effects of Zr impurity on microscopic behavior of Hf metal

Hf metal with ∼ 3 wt% Zr impurity has been reinvestigated by perturbed angular correlation (PAC) spectroscopy using a LaBr₃(Ce)–BaF₂ detector set up to understand the microscopic behavior of this metal with temperature. From present measurements, five quadrupole interaction frequencies have been found at room temperature where both pure hcp fraction (∼33%) with 12 nearest neighbor Hf surrounding the probe ¹⁸¹Hf atom and the probe–impurity fraction (∼33%) corresponding to 11 nearest neighbor Hf plus one dissimilar Zr atom are clearly distinguished. At room temperature, the results for quadrupole frequency and asymmetry parameter are found to be ω_Q=51.6(4) Mrad/s, η=0.20(4) for the impurity fraction and ω_Q=46.8(2) Mrad/s, η=0 for the pure fraction with values of frequency distribution width δ=0 for both components. At 77 K, only 1 NN Zr impurity (∼93%) and pure hcp (∼7%) components have been found with a value of δ ∼ 10% for the impurity fraction. A drastic change in microstructural configuration of Hf metal is observed at 473 K where the impurity fraction increases to ∼ 50% and the pure hcp fraction reduces to ∼ 15% with abrupt changes in quadrupole frequencies for both components. The pure fraction then increases with temperature and enhances to ∼50% at 973 K. In the temperature range 473–973 K, quadrupole frequencies for both components are found to decrease slowly with temperature. Using the Arrhenius relation, binding energy (B) for the probe–impurity pair and the entropy of formation are measured from temperature dependent fractions of probe–impurity and pure hcp in the temperature range 473–773 K. The three other minor components found at different temperatures are attributed to crystalline defects.     

Sintering kinetic measurement of nickel nanoparticle agglomerates by electrical mobility classification

The gas-phase sintering kinetics of nickel nanoparticle agglomerates was investigated by a two step electrical mobility classification. The first electrostatic classifier sorted the agglomerated mono-area nickel nanoparticles generated by pulsed laser ablation, and then the subsequent heating process created the sintered nickel nanostructures. The second electrostatic classifier combined with the condensation nucleus counter scanned the shrinkage of the agglomerated mono-area nickel nanoparticles due to the sintering process. The change in the mono-area particle mobility size measured by the electrical mobility classification technique was compared with the results of the existing coalescence model to extract the kinetic parameters for the sintering of nickel particles. The optimum activation energy found in this study was ∼63 kJ/mol, which falls between the diffusion of nickel atoms (∼49 kJ/mol) and the migration and coalescence of nickel particles (∼78 kJ/mol).     

Performance improvement of ZnO/P3HT hybrid UV photo-detector by interfacial Au nanolayer

In this study, a hybrid ultraviolet (UV) photo detector comprising of hydrothermally grown highly oriented Zinc Oxide nanorod arrays (ZnO NRAs) and Poly(3-hexylthiophene-2,5-diyl) (P3HT) as an active layer was fabricated and characterized. These hybrid photo detectors demonstrated a high rectification ratio (∼117) and responsivity of 10.7 A/W at −2  V under incident light of wavelength 325 nm. Further to investigate the effect of surface plasmon property of metal nanoparticles on the performance of hybrid UV photo detectors, ZnO NRAs were capped with dc sputtered gold (Au) metal nanolayer (∼5 nm) at the ZnO-P3HT interface, prior to coating P3HT layer on top of it. It was found out that upon Au coating the absorption of the ZnO was enhanced partly in the ultraviolet and visible region. In consequence the rectification ratio and responsivity of the hybrid photo detector was enhanced drastically from 117 to 1167 and 10.7 to 17.7 A/W respectively. Interestingly the reduction in dark current was observed on Au coating and it was revealed that Au nanoparticles play a key role in enhancing the performance of the hybrid photo detectors.     

Dielectric relaxation of ZnO nanostructure synthesized by soft chemical method

Thioglycerol capped nanoparticles of ZnO have been prepared in methanol through chemical technique. Nanostructures of the prepared ZnO particles have been confirmed through X-ray diffraction measurement. The Debye–Scherrer formula is used to obtain the particle size. The average size of the prepared ZnO nanoparticles is found to be 50 nm. The frequency-dependent dielectric dispersion of the sample is investigated in the temperature range from 293 to 383 K and in a frequency range from 100 Hz to 1 MHz by impedance spectroscopy. An analysis of the complex permittivity (ε′ and ε′′) and loss tangent (tan δ) with frequency is performed assuming a distribution of relaxation times. The frequency-dependent maxima of the imaginary part of impedance are found to obey Arrhenius law with activation energy ∼1 eV. The scaling behavior of dielectric loss spectra suggests that the relaxation describes the same mechanism at various temperatures. The frequency-dependent electrical data are analyzed in the framework of conductivity and modulus formalisms. The frequency-dependent conductivity spectra obey the power law.     

Synthesis,characterization and magnetic properties of lightly doped La2−xSrxCuO4 (x = 0.04) nanoparticles

Lightly doped La_2−xSr_xCuO₄ (x = 0.04) nanoparticles with different particle sizes have been successfully prepared by a sol–gel method and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared transmission (IR) spectra and superconducting quantum interference device (SQUID) magnetometer. All samples are single phase and have an orthorhombic unit cell. As the particle size reduces, it is found that the IR band at around 685 cm⁻¹ corresponding to the in-plane Cu–O asymmetrical stretching mode shifts to higher frequency and the magnetization exhibits a large enhancement at low temperature. The magnetic susceptibility of all samples follows a modulated Curie law between ∼20 K and ∼100 K and the Curie constant displays a strong dependence on the particle size. It is suggested that as the particle size decreases surface effects should play an important role in the magnetic properties of the nanoparticles.     

Influence of Cu doping on the microstructure,optical properties and photoluminescence features of Cd0.9Zn0.1S nanoparticles

Cd_0.9−xZn_0.1Cu_xS (0≤x≤0.06) nanoparticles were successfully synthesized by a conventional chemical co-precipitation method at room temperature. Crystalline phases and optical absorption of the nanoparticles have been studied by X-ray diffraction (XRD) and UV–visible spectrophotometer. XRD confirms the phase singularity of the synthesized material, which also confirmed the formation of Cd–Zn–Cu–S alloy nanocrystals rather than separate nucleation or phase formation. Elemental composition was examined by the energy dispersive X-ray analysis and the microstructure was examined by scanning electron microscope. The blue shift of absorption edge below Cu=2% is responsible for dominance of Cu⁺ while at higher Cu concentration dominated Cu²⁺, d–d transition may exist. It is suggested that the addition of third metal ion (Cu²⁺/Cu⁺) is an effective way to improve the optical property and stability of the Cd_0.9Zn_0.1S solid solutions. When Cu is introduced, stretching of Cd–Zn–Cu–S bond is shifted lower wave number side from 678 cm⁻¹ (Cu=0%) to 671 cm⁻¹ (Cu=6%) due to the presence of Cu in Cd–Zn–S lattice and also the size effect. The variation in blue band emission peak from 456 nm (∼2.72 eV) to 482 nm (∼2.58 eV) by Cu-doping is corresponding to the inter-band radiation combination of photo-generated electrons and holes. Intensity of red band emission centered at 656 nm significantly increased up to Cu=4%; beyond 4% it is decreased due to the quenching of Cu concentration.     

Silver nanoparticle in situ growth within crosslinked poly(ester-co-styrene) induced by UV irradiation: aggregation control with exposure time

Silver nanoparticles (NPs) were photogenerated in situ in crosslinked poly(ester-co-styrene) resins (self-standing films and monoliths) by irradiating the samples with UV light. Addition of the silver salt solution did not interfere in the resin curing process and silver reduction was not detected during sample crosslinking. The samples were characterized by absorption spectroscopy and transmission electron microscopy. The initially broad and asymmetric surface plasmon resonance band was narrowed and blue-shifted as the exposure time to UV light was increased. Samples illuminated up to 120 min have an average particle size near 9.0 nm; a decrease to ∼5.0 nm was observed for longer exposure times up to 790 min. The asymmetric surface plasmon resonance band was due to particle aggregation; higher irradiation times led to a uniform particle distribution within the polymer matrix.     

Fragmentation of elongated-shaped ZnO nanostructures into spherical particles by swift ion impact

This work reports on the fragmentation of rod-shaped ZnO nanostructures into spherical nanoparticles under 120 MeV Ag⁹⁺ swift ion irradiation. The visual evidence of the irradiation induced morphological change has been witnessed through electron microscopic studies. Typically, rods of 50 nm length and 21 nm diameter have transformed into particles of smaller dimension. Conversely, X-ray diffraction studies have revealed the lowering of crystallite size from 21.5 nm to 9 nm and an increase in microstrain by 11 times. Further, spectroscopic results, such as, significant blue shift (∼24 cm⁻¹) in vibrational features of Zn–O bonding, increase in native defect concentration in the nanostructures etc. also favor the irradiation led modification of nanostructures. It was anticipated that, dislodging and recrystallization of the constituent atoms of the elongated systems, as a consequence of suppression of the cohesive energy (owing to enormous energy deposition) caused by energetic ion irradiation, is chiefly responsible for the evolution of spherical nanoparticles.     

Magnetic properties of iron nanoparticles in a polymer film

We systematically synthesized self-aggregated iron nanoparticles in the perfluorinated sulfo-cation membrane (MF-4SK) by ion-exchange method. Our experimental results show that iron nanoparticles in MF-4SK exhibit superparamagnetic properties above the blocking temperature. Field-cooled and zero-field-cooled magnetization data show the blocking temperature, T_B≅120 K for the iron concentration of 5×10¹⁹ atoms per 1 g of polymer film at 500 Oe applied field. This result is well matched with the calculation based on the temperature dependence of the coercivity, which shows T_B≅110 K, with the zero temperature coercivity (H_C0) ≅ 420 Oe. The radius of the typical iron particle is determined to be ∼2 nm from transmission electron microscopy (TEM), showing good agreement with the value acquired by Langevin function fit. These experimental evidences suggest that iron nanoparticles in the polymer film obey a single-domain theory.     

In situ SEM,TEM and AFM studies of the antimicrobial activity of lemon grass oil in liquid and vapour phase against Candida albicans

Inhibition of Candida albicans growth was shown by lemon grass oil (LGO) and lemon grass oil vapour (LGO vapour) at 288 μg/ml and 32.7 μg/ml concentration, respectively. The assessment of cell damage by LGO and LGO vapour was done through scanning electron microscope (SEM), transmission electron microscope (TEM) and atomic force microscope (AFM) observations. SEM analysis showed complete rupture of C. albicans cells treated with LGO vapour while in those treated with LGO in broth, only shrinkage was observed. TEM study showed the alterations in morphology upon treatment with LGO while complete degradation of the Candida cells was observed in case of LGO vapour. Further three dimensional morphological changes and roughness of the cells have also been evaluated with AFM after the treatment with LGO & LGO vapour. Roughness (root mean square value) was significantly higher in control C. albicans cells (211.97 nm) than LGO (143 nm) and LGO vapour (5.981 nm) treated cells. The results for the first time demonstrate relatively higher efficacy of LGO vapours for inhibition and cellular damage of C. albicans cells as compared to the LGO in liquid phase. This suggests the potential application of LGO vapour phase against infections caused by C. albicans.     

Large-scale synthesis and magnetic properties of cubic CoO nanoparticles

We present the synthesis, microstructural and magnetic characterization of cubic CoO nanoparticles with well-controlled size and shape. The as-synthesized CoO nanoparticles are stable because of the organic coating that occurred in situ. The Néel temperature is 225 and 280 K for the 42 and 74 nm CoO particles, respectively. The CoO nanoparticles exhibit anomalous magnetic properties, such as large moments, coercivities and loop shifts. These results provide evidence for the formation of spin compensated random system in CoO. The structurally distorted and magnetically disordered surface layer ferromagnetic phase played an important role in the magnetic behavior of CoO nanoparticles. The smaller is the particle size, the stronger is the contribution of the ferromagnetic phase and the more is the surface layer helpful to enhance the observed coercivity and the exchange bias.     

Investigation of magnetic properties of interacting Fe2O3 nanoparticles

The magnetic properties of Fe₂O₃ nanoparticles (average diameter ∅≅3 nm) in alumina (68% Fe₂O₃ in weight) have been investigated by magnetization measurements. The results indicate a superparamagnetic behavior of interacting particles, which block with decreasing temperature (the zero-field-cooled susceptibility shows a maximum at T≅145 K) with a distribution of relaxation times. A change of magnetic regime is observed below ∼60 K, due to the increasing interparticle interactions and local surface anisotropy.     

Improved short-circuit photocurrent densities in dye-sensitized solar cells based on ordered arrays of titania nanotubule electrodes

We report on the synthesis of highly ordered arrays of titania nanotubules and their applications in enhanced photoelectrochemical cells. Ordered arrays of titania nanotubules of ∼120 nm external diameter, ∼100 nm internal diameter, and ∼5 μm length were fabricated on transparent conductive oxide (TCO) glass substrates by sol–gel processes using in-house prepared anodic alumina templates. After thermal bonding and template removal, the resultant nanotubule structures were applied in dye-sensitized solar cells (DSCs). Overall photoconversion efficiency of nearly 4.8% was achieved with Ru-bipyridine dye, N719, and iodolyte liquid electrolyte. This remarkable performance, for electrodes only ∼5 μm thick, is attributed to an unexpectedly high short-circuit photocurrent density of 16 mA/cm² for masked cells and up to 17 mA/cm² for unmasked cells. The enhanced short-circuit photocurrent (J_sc) is attributed to the high surface area (roughness factor ca. 1207) of the nanotubules and thus improved dye adsorption to the electrodes. The improved J_sc is also attributed to the parallel and vertical orientation of the nanostructures and thus to a well-defined electron diffusion path.     

Irradiation induced modifications in morphology and magnetic property of Mn/Si structure

Mn films of ∼50 nm has been deposited by electron beam evaporation technique on cleaned and etched Si [(1 0 0), 8–10 Ω cm] substrates to realize a Mn/Si interfacial structures. The structures have been irradiated from energetic (∼100 MeV) ion beam from Mn side. The irradiated and unirradiated structures have been characterized from atomic force microscopy, X-ray diffractometry, magnetic force microscopy, and vibrating sample magnetometer facilities. It has been found that surface/interfacial granular silicide phases (of Mn_xSi_y) are formed before and after the irradiation with a irradiation induced modifications of surface morphology and magnetic property. The surface/interface roughness has been found to increase on the irradiation from the atomic force microscopy data. The magnetic property on the irradiation shows an interesting and significant feature of an increased coercivity and a ferromagnetic like behavior in the Mn–Si structure. The observed increased coercivity has been related to the increased roughness on the irradiation. The ferromagnetism after the irradiation is a curious phenomenon which seems due to the formation of Mn–C–Si compound from the carbon dissolved in silicon.     

Influence of substrate temperature on physical properties of sprayed Zn0.85Mn0.15O films

Zn_1−xMn_xO thin films have been synthesized by chemical spray pyrolysis at different substrate temperatures in the range, 250–450 °C for a manganese composition, x = 15%, on corning 7059 glass substrates. The as-grown layers were characterized to evaluate their chemical and physical behaviour with substrate temperature. The change of dopant level in ZnO films with substrate temperature was analysed using X-ray photoelectron spectroscope measurements. The X-ray diffraction studies revealed that all the films were strongly oriented along the (0 0 2) orientation that correspond to the hexagonal wurtzite structure. The crystalline quality of the layers increased with the increase of substrate temperature up to 400 °C and decreased thereafter. The crystallite size of the films varied in the range, 14–24 nm. The surface morphological studies were carried out using atomic force microscope and the layers showed a lower surface roughness of 4.1 nm. The optical band gap of the films was ∼3.35 eV and the electrical resistivity was found to be high, ∼10⁴ Ω cm. The films deposited at higher temperatures (>350 °C) showed ferromagnetic behaviour at 10 K.     

High-density uniformly aligned silicon nanotip arrays and their enhanced field emission characteristics

High-density (∼10⁸/cm²), uniformly aligned silicon nanotip arrays are synthesized by a plasma-assisted hot-filament chemical vapor deposition process using mixed gases composed of hydrogen, nitrogen and methane. The silicon nanotips grow along 〈112〉, and are coated in situ with a ∼3 nm thick amorphous carbon film by increasing the methane concentration in the source gases. In comparison to the uncoated silicon nanotips arrays, the coated tips have enhanced field emission properties with a turn-on field of 1.6 V/μm (for 10 μA/cm²) and threshold field of 3 V/μm (for 10 mA/cm²), suggesting their potential applications for flat panel displays.     

Effect of thin aluminum interlayer on growth and microstructure of carbon nanotubes

The aluminum (Al) interlayer with various thicknesses ranging from 0.75 to 6 nm was deposited on silicon (Si) substrates prior to the deposition of ultra-thin iron (Fe) catalyst for the growth of carbon nanotubes. In this paper we report the effect of ultra-thin Al interlayer on the growth of multiwalled carbon nanotubes (MWCNTs). The SEM was used to examine the microstructures of nanotubes. We observed as the Al interlayer thickness increases the height of nanotube decreases. Raman spectra of MWCNT showed typical D and G peaks at ∼1345 cm⁻¹ and ∼1575 cm⁻¹, respectively. The XPS revealed the presence of Al and Fe on the top of CNT surface which were further supported by TEM. The high resolution TEM results also revealed bamboo like CNTs with diameter ∼10–40 nm.     

Sonochemical effect on size reduction of CaCO3 nanoparticles derived from waste eggshells

A novel combination of mechanochemical and sonochemical techniques was developed to produce high-surface-area, bio-based calcium carbonate (CaCO₃) nanoparticles from eggshells. Size reduction of eggshell achieved via mechanochemical and followed by sonochemical method. First, eggshells were cleaned and ground, then ball milled in wet condition using polypropylene glycol for ten hours to produce fine particles. The ball milled eggshell particles were then irradiated with a high intensity ultrasonic horn (Ti-horn, 20 kHz, and 100 W/cm²) in the presence of N,N-dimethylformamide (DMF); decahydronaphthalene (Decalin); or tetrahydrofuran (THF). The ultrasonic irradiation times varied from 1 to 5 h. Transmission electron microscopic (TEM) studies showed that the resultant particle shapes and sizes were different from each solvent. The sonochemical effect of DMF is more pronounced and the particles were irregular platelets of ～10 nm. The BET surface area (43.687 m²/g) of these nanoparticles is much higher than that of other nanoparticles derived from eggshells.