Preparation of triethylamine stabilized silver nanoparticles for low-temperature sintering

In this article, silver nanoparticles were synthesized by chemical reduction from silver nitrate using triethylamine as the protecting and reducing agents simultaneously. The average size of the silver nanoparticles was about 2.10–4.65 nm, which allowed low-temperature sintering of the metal. X-ray diffraction (XRD), thermogravimetric analysis (TGA), and energy dispersive spectrometric (EDS) analysis results indicate that silver nitrate has been converted to silver nanoparticles completely. Using a 20 wt% silver nanoparticles suspension with thermal treatment at 150 °C, silver films with a resistivity of 8.09 × 10⁻⁵ Ω cm have been produced, which is close to the resistivity of bulk silver.     

Synthesis of transparent BaTiO3 nanoparticle/polymer composite film using DC field

Transparent BaTiO₃ nanoparticle/polymer composite films were synthesized from titanium-organic film and barium ion in aqueous solution under direct current (DC) field. Titanium-organic precursor was synthesized from titanium isopropoxide, acetylacetone and methacrylate derivative. The UV treatment was effective to increase the anti-solubility of the titanium-organic film during DC processing. BaTiO₃ nanoparticles were crystallized in the precursor films on stainless substrates without high temperature process, as low as 40°C. The crystallite size of BaTiO₃ increased with increasing reaction temperature from 40 to 50 °C at 3.0 V/cm. BaTiO₃ nanoparticles also grew in size with increasing reaction time from 15 min to 45 min at 3.0 V/cm and 50 °C. Transparent BaTiO₃ nanoparticle/polymer films were synthesized on stainless substrates at 3.0 V/cm and 50°C for 45 min.     

Photoconductivity studies on amorphous and crystalline TiO<Subscript>2</Subscript> films doped with gold nanoparticles

In this work, amorphous and crystalline TiO₂ films were synthesized by the sol–gel process at room temperature. The TiO₂ films were doped with gold nanoparticles. The films were spin-coated on glass wafers. The crystalline samples were annealed at 100°C for 30 minutes and sintered at 520°C for 2 h. All films were characterized using X-ray diffraction, transmission electronic microscopy and UV-Vis absorption spectroscopy. Two crystalline phases, anatase and rutile, were formed in the matrix TiO₂ and TiO₂/Au. An absorption peak was located at 570 nm (amorphous) and 645 nm (anatase). Photoconductivity studies were performed on these films. The experimental data were fitted with straight lines at darkness and under illumination at 515 nm and 645 nm. This indicates an ohmic behavior. Crystalline TiO₂/Au films are more photoconductive than the amorphous ones.     

Study of field emission and dielectric properties of AlN films prepared by DC sputtering technique at different substrate temperatures

Nanocrystalline AlN thin films were prepared via DC sputtering technique at different substrate temperature. The crystal orientation and particle size of aluminum nitride thin films were investigated by XRD analysis. Study indicated that the sample contained pure phase hexagonal AlN nanoparticles with a single peak corresponding to the (100) planes. The peak at 665 cm⁻¹ in the FTIR spectrum of film was assigned to the LO phonon of hexagonal AlN. The particle size of the film, prepared at substrate temperature 200°C was about 9.5 nm, as investigated by atomic force microscope. Field emission study indicated that it can be used as a good field emitter. Turn-on field (E_to) of 15.02 V/μm was observed for the AlN films synthesized at substrate temperature 200°C. Dielectric constant of the AlN film was found nearly independent of frequencies in the measured frequency range 1 KHz to 1 MHz, i.e. in the audio frequency range. The values of dielectric constant (ε) were 10.07, 9.46 and 8.65 for the film prepared at 70°C, 150°C and 200°C, respectively, at frequency 1 KHz.     

Photoluminescence characteristics of ZnGa2O4 thin films prepared by chemical solution method

Zinc gallate (ZnGa₂O₄) thin film phosphors have been formed on ITO glass substrates by a chemical solution method with starting materials of zinc acetate dihydrate, gallium nitrate hydrate and 2-methoxiethanol as a solution. The thin films were firstly dried at 100 °C and fired at 500 °C for 30 min and then, annealed at 500 °C and 600 °C for 30 min under an annealing atmosphere of 3% H₂/Ar. XRD patterns of the thin film phosphors showed (311) and (220) peak indicating ZnGa₂O₄ crystalline phase in which all the (311) peaks of the film phosphors synthesized on ITO glass and soda-lime glass revealed high intensity with increasing annealing temperature from 500 °C to 600 °C. The ZnGa₂O₄ thin film phosphors represented marked change in AFM surface morphologies according to an annealing temperature under an annealing atmosphere (3% H2/Ar). The film phosphor, annealed at 600 °C, showed the embossed pattern with relatively regular spacing in AFM surface morphology. The ZnGa₂O₄ thin film phosphors formed on ITO glass, which were annealed at different temperatures and showed distinctive spectra with peak wavelengths of 434 nm and 436 nm in the blue emission region.     

In situ growth of silver nanoparticles in mesoporous silica by spray pyrolysis

Silver-dispersed mesoporous silica was in situ synthesized in aerosol phase. The solidification of silica was catalyzed in the presence of the silver, which increased the order and d values of the mesophase at given reactor temperature. Silver nanoparticles grew confined in the pores when the atomic % of silver to Si was below 10 and the pore wall turned to be impermeable above 400 °C. Silver permeated through the pore wall below 400 °C to grow freely in the carrier gas. The mesophase deteriorated using spray pyrolysis above 800 °C due to the further densification of silica, or above 10 at.% of silver due to the excessive growth within the phase. The highest dispersion of silver ~4 nm in diameter with the highest order of the mesoporosity was obtained at 600 °C with 5 at.% silver. Calcination following the spray pyrolysis further densified the silica phase to freeze the growth of silver particles as well as lower the d value of the mesophase.     

Thermal transformations in soils studied by Mössbauer spectroscopy and x-ray diffraction

Mossbauer spectroscopy and X-ray diffraction techniques were used to investigate the iron oxides and other mineral phase developments in calcareous and noncalcareous soil samples after firing at ≈ 1000°C. Well crystalline haematite with larger particle size was produced in the fired non-calcareous soil. On the other hand, while goethite in the strongly calcareous natural material was transformed into haematite at the oven drying temperature, non of the latter was detected after firing at 1050°C. This could be related to the reaction between CaO, quartz and aluminosilicates at 800°C to produce calcium aluminosilicates which may have hindered the growth of haematite above this temperature.     

A newly developed Fe-doped calcium sulfide nanoparticles with magnetic property for cancer hyperthermia

In this study, a magnetic iron-doped calcium sulfide (Fe–CaS) nanoparticle was newly developed and studied for the purpose of hyperthermia due to its promising magnetic property, adequate biodegradation rate, and relatively good biocompatibility. Fe–CaS nanoparticles were synthesized by a wet chemical co-precipitation process with heat treatment in a N₂ atmosphere, and were subsequently cooled in N₂ and exposed to air at a low temperature. The crystal structure of the Fe–CaS nanoparticles was similar to that of the CaS, which was identified by an X-ray diffractometer (XRD). The particle size was less than 40 nm based on a Debye–Scherrer equation and transmission electron microscope (TEM) examination. Magnetic properties obtained from the SQUID magnetometer demonstrated that the synthesized CaS was a diamagnetic property. Once the Fe ions were doped, the synthesized Fe–CaS converted into paramagnetism which showed no hysteresis loop. Having been heated above 600 °C in N₂, the Fe–CaS showed a promising magnetic property to produce enough energy to increase the temperature for hyperthermia. 10 mg/ml of the Fe–CaS was able to generate heat to elevate the media temperature over 42.5 °C within 6 min. The area of the hysteresis loop increased with the increasing of the treated temperature, especially at 800 °C for 1 h. This is because more Fe ions replaced Ca ions in the lattice at the higher heat treatment temperature. The heat production was also increasing with the increasing of heat treatment temperature, which resulted in an adequate specific absorption ratio (SAR) value, which was found to be 45.47 W/g at 37 °C under an alternative magnetic field of f = 750 KHz, H = 10 Oe. The in vitro biocompatibility test of the synthesized Fe–CaS nanoparticles examined by the LDH assay showed no cytotoxicity to 3T3 fibroblast. The result of in vitro cell hyperthermia shows that under magnetic field the Fe–CaS nanoparticles were able to generate heat and kill the CT-26 cancer cells significantly. We believe that the developed Fe–CaS nanoparticles have great potential as thermo-seeds for cancer hyperthermia in the near future.     

Surface-enhanced absorption by self-organized silver films with aciniform-like nanoaggregates at elevated temperatures

Morphological evolution of silver nanocomposite films prepared by the wet colloidal route and surface-enhanced phenomena on aggregate nanostructures evolved during annealing were investigated. Dramatic changes in morphologies of particles and pores incurred by rearragement, coarsening, premelting, and dewetting of the silver clusters at different concentrations (i.e., mass thicknesses). At a higher mass thickness, the morphological transitions from self-organized nanoaggregates with aciniform pattern at 300 °C to elongated and coarsened particles with circular holes at 400 °C to island clusters at 500 °C occurred in the films. The peculiar absorption with a much redder and broader surface plasmon feature, which gone far beyond the theoretical prediction, induced by the formation of aciniform nanoaggregates embedded in the porous polymer matrix at a critical mass thickness of 9.6 nm during partial degradation of the PVP polymer and rearrangement of silver clusters at 300 °C. The surface-enhanced absorption was dramatically reduced by the elemination of the aggregate nanostructures and the spontaneous formation of the silver nanoisland film at the dewetting temperature of 500 °C.     

Efficient fabrication of transparent antimicrobial poly(vinyl alcohol) thin films

We have explored in situ synthesis of Ag nanoparticles in transparent PVA films in view of increasing areas of application of those films. The two-step procedure consists of ion incorporation in the matrix and subsequent thermal reduction. Smooth and transparent PVA films containing Ag nanoparticles of 5–20 nm were fabricated by this approach. The optical property of the films and the size of metal nanoparticles could be controlled by changing the reaction conditions. By increasing heating temperature, the absorbance and wavelength of surface plasmon resonance (SPR) of the composite film increased, and nanoparticles with larger particle sizes and broader size distributions were obtained. In the temperature range of 130–170 °C, the wavelength of SPR increased with increasing the AgNO₃ concentration. At 190 °C, however, the wavelenght of SPR blue-shifted initially when the AgNO₃ concentration increased from 10 to 80 mmol/L, and red-shifted thereafter. The composite films showed excellent antimicrobial performance toward bacteria such as Escherchia coli. Such hybrids afford very effective and environment-friendly antimicrobial surface coatings.     

Synthesis,structure stability and magnetic properties of nanocrystalline Ag–Ni alloy

Silver–nickel alloy nanoparticles with an average size of 30–40 nm were synthesized by chemically reducing the mixture of silver and nickel salts using sodium borohydride. The structure and the magnetic properties of the alloy samples with different compositions were investigated. The phase stability of the material was analysed after annealing the sample in vacuum at various temperatures. The material exhibits single fcc phase which is stable up to 400 °C and Ni precipitation sets in when the sample is annealed to 500 °C. The thermal analysis using DSC was carried out to confirm the same. The alloy compositions are found to be in close correlation with the metal salt ratios in the precursors. The synthesized samples exhibit weak paramagnetic to ferromagnetic behaviour. The magnetic measurements reveal that by adjusting the precursor ratio, the Ni content in the material can be altered and hence its magnetic properties tailored to suit specific requirements. The formation of Ag–Ni alloy is confirmed by the observed Curie temperature from the magneto thermogram. Annealing the sample helps to produce significant enhancement in the magnetization of the material.     

Synthesis and photoluminescence properties of silver nanowires

Silver nanowires of 50–190 nm in diameters along with silver nanoparticles in the size range of 60–200 nm in prismatic and hexagonal shapes are synthesized through chemical process. The lengths of the silver nanowires lie between 40 and 1000 μm. The characterizations of the synthesized samples are done by X-ray diffraction (XRD), scanning electron microscopy (SEM) and UV–visible absorption spectroscopy. The syntheses have been done by using two processes. In the first process, relatively thicker and longer silver nanowires are synthesized by a soft template liquid phase method at a reaction temperature of 70 °C with methanol as solvent. In the second process, thinner silver nanowires along with silver nanoparticles are prepared through a polymer mediated polyol process at a reaction temperature of 210 °C with ethylene glycol as solvent. The variations of photoluminescence (PL) emission from the silver nanocluster dispersed in methanol as well as in ethylene glycol are recorded at room temperature under excitation wavelengths lying in between 300 and 414 nm. The blue–green PL emission is observed from the prepared samples and these emissions are assigned to radiative recombination of Fermi level electrons and sp- or d-band holes.     

Luminescence in Colorless,Transparent, Thermally Stable Thin Films of Eu<Superscript>3+</Superscript> and Tb<Superscript>3+</Superscript> β-diketonates in Hybrid Inorganic–Organic Zinc-based Sol–Gel Matrix

Luminescent zinc-based hybrid inorganic–organic films with rare--earth (RE) complexes have been prepared using a non-alkoxide sol–gel process. The films were fabricated by the dip-coating method starting from zinc acetate dihydrate, rare earth chloride, lactic acid as hydrolytic catalyst, and anhydrous ethanol. The β-diketones thenoylltrifluoroacetone (Httfa) and dibenzoylmethane (Hdbm) were used as ligands to Eu³⁺ and Tb³⁺, respectively. After deposition of the first layer, the films were fired at temperatures between 50 and 300 °C, in air. Photophysical properties such as excitation, emission and emission, lifetimes were determined for the films obtained in different conditions. Eu³⁺/ttfa and Tb³⁺/dbm films fired at 300 and 250 °C, respectively, are still transparent and gave rise to intense emission when excited through the ligand (antenna effect).     

Nonlinear optical properties of nanometer-size silver composite azobenzene containing polydiacetylene film

Diacetylene monomer containing p-nitrophenyl azobenzene moiety (NADA) was synthesized. Silver nanoparticles with different concentrations were adulterated in the above polymerized NADA (PNADA) films and the third-order nonlinear optical properties were investigated in detail. UV–vis spectra and transmission electron microscopy were used to confirm the formation of PNADA/Ag nanocomposite films. The silver nanoparticles (average size of 10 nm) were well dispersed in the polymer films. The value of the nonlinear refractive index n ₂ for PNADA films (8.48×10⁻¹⁵ cm²/W) was much higher than that of pure polydiacetylene films. Further, the introduction of silver nanoparticles into the PNADA polymer films led to the further enhancement of nonlinear optical properties. The maximum value of n ₂ for PNADA/Ag nanocomposite films could be 11.6×10⁻¹⁵ cm²/W. This enhancement should be ascribed to the surface plasmon resonance of silver nanoparticles.     

Efficient synthesis of ZnO nanoparticles,nanowalls, and nanowires by thermal decomposition of zinc acetate at a low temperature

ZnO nanoparticles, nanowires, and nanowalls were synthesized rapidly on Si via thermal decomposition of zinc acetate by a modified chemical vapor deposition at a low substrate temperature of 200–250°C for the first time. The diameters of the synthesized nanoparticles and nanowires are around 100 and 30 nm, respectively, and the thickness of nanowalls is around 20 nm. High-resolution transmission electron microscopy shows that the nanowires as well as nanowalls are single-crystalline, and the nanoparticles are highly-textured poly-crystalline structures. Room-temperature photoluminescence spectra of the nanostructures show strong ultraviolet emissions centered at 368–383 nm and weak violet emissions at around 425 nm, indicating good crystal quality. The study provides a simple and efficient route to synthesize ZnO diverse nanostructures at low temperature.     

Fusarium solani: a novel biological agent for the extracellular synthesis of silver nanoparticles

We report extracellular biosynthesis of silver nanoparticles by Fusarium solani (USM-3799), a phytopathogen causing disease in onion, when challenged with 1 mM silver nitrate (AgNO₃). The formation of nanoparticles was characterized by visual observation followed by UV–Vis spectrophotometric analysis, which showed a peak at about 420 nm, which is very specific for silver nanoparticles. Further analysis carried out by Fourier Transform Infrared Spectroscopy (FTIR), provides evidence for the presence of proteins as capping agent, which helps in increasing the stability of the synthesized silver nanoparticles. Transmission Electron Microscopy (TEM) investigations confirmed that silver nanoparticles were formed. The synthesized silver nanoparticles were found to be polydispersed, spherical in the range of 5–35 nm with average diameter of 16.23 nm. Extracellular synthesis of nanoparticles could be highly advantageous from the point of view of synthesis in large quantities and easy downstream processing.     

The production of Sr hexaferrite thick films by screen printing

Hydrothermally synthesised Sr hexaferrite (HT-SrM) powder with a distinct plate-like shape and conventional Sr hexaferrite (c-SrM) powder were used to screen print SrM thick films on alumina substrates. In the case of the HT-SrM thick films, a very strong perpendicular magnetic anisotropy has been observed with remanence values of up to 42±2 J/T kg for the perpendicular direction and 15±1 J/T kg for the in-plane direction, and with coercivities of around 159±8 kA/m for both directions when fired at 1300°C. When fired at 1150°C, the remanences were 49±2 and 27±2 J/T kg for the two directions with a higher coercivity of 247±8 kA/m for both directions. The SEM micrographs showed that the platelet grains in the printed films lay with their flat surfaces on the substrate and XRD results revealed that the c-axis of the grains oriented perpendicularly to the film surface. The (0 0 8) plane, which is, for a random oriented sample, a very weak peak, appeared as the strongest in the XRD pattern for the films. EDX and XRD studies indicated significant reaction at the interfaces between the film and the substrate when the sintering temperature was raised to 1350°C.For the SrM thick films obtained from planetary milled ultrafine Sr hexaferrite and conventional Sr hexaferrite powder, a slight in-plane anisotropy could be observed with a coercivity of 318±8 kA/m.     

Fabrication and optical study of Ag@SnO<Subscript>2</Subscript> core-shell structure nanoparticle thin films

Ag@SnO₂ core-shell nanoparticles dispersed in poly-(vinyl) alcohol films were fabricated on glass substrate by employing a dip-coating technique. Synthesis of Ag@SnO₂ nanoparticles with core-shell morphology is carried out by a soft-chemical technique in aqueous phase at 60°C. Formation of core-shell structure is monitored by the red-shift of the surface plasmon band of Ag nanoparticles (from 390 to 410 nm) in the UV-visible spectrum. These nanoparticles are deposited on the glass substrate. The structure and morphology of these films were investigated by X-ray diffraction technique and field-emission transmission electron microscopy, respectively. Optical properties of these pseudo-solids were studied by UV-visible spectroscopy. Surface plasmon spectrum of the core-shell nanoparticles film remained unaltered with increase in the number of layers. However, silver nanoparticles films have shown peak broadening and development of additional peaks with increase in the number of layers. Our investigations showed that the surface plasmon band of the silver nanoparticles could be preserved by controlled deposition of the tin dioxide shell.     

Synthesis,deposition and characterization of tin selenide thin films by thermal evaporation technique

Tin selenide alloy was synthesized by following simple chemical reaction method, at comparatively lower temperature of 100 °C, from alkaline medium using SnCl₂.2H₂O and selenium as source materials. Powder X-ray diffraction analysis reveals that the particle size of the synthesized product is in nanometer scale. Using the reaction product as source material, the SnSe films were deposited on glass substrates at room temperature, 150 °C, 250 °C, 350 °C and 450 °C. Structural, elemental, optical, surface morphological and electrical properties of the as deposited films were studied by X-ray diffraction, Energy Dispersive X-ray Analysis, UV-Vis-NIR, Scanning Electron Microscopy and Hall effect measurement techniques and the relevant details have been obtained.     

Effect of melt compounding temperature on dielectric relaxation and ionic conduction in PEO–NaClO<Subscript>4</Subscript>–MMT nanocomposite electrolytes

Polymer nanocomposite electrolytes (PNCEs) of poly(ethylene oxide) and sodium perchlorate monohydrate complexes with montmorillonite (MMT) clay up to 20 wt.% MMT concentration of poly(ethylene oxide) (PEO) are synthesized by melt compounding technique at melting temperature of PEO (∼70 °C) and NaClO₄ monohydrate (∼140 °C). Complex dielectric function, electric modulus, alternating current (ac) electrical conductivity, and impedance properties of these PNCEs films are investigated in the frequency range 20 Hz to 1 MHz at ambient temperature. The direct current conductivity of these materials was determined by fitting the frequency-dependent ac conductivity spectra to the Jonscher power law. The PNCEs films synthesized at melting temperature of NaClO₄ monohydrate have conductivity values lower than that of synthesized at PEO melting temperature. The complex impedance plane plots of these PNCEs films have a semicircular arc in upper frequency region corresponding to the bulk material properties and are followed by a spike in the lower frequency range owing to the electrode polarization phenomena. Relaxation times of electrode polarization and ionic conduction relaxation processes are determined from the frequency values corresponding to peaks in loss tangent and electric modulus loss spectra, respectively. A correlation is observed between the ionic conductivity and dielectric relaxation processes in the investigated PNCEs materials of varying MMT clay concentration. The scaled ac conductivity spectra of these PNCEs materials also obey the ac universality law.