Preparation and characterization of carbon aerogel microspheres by an inverse emulsion polymerization

Carbon aerogel (CA) microspheres have been successfully synthesized by an inverse emulsion polymerization and characterized by scanning electron microscopy (SEM), N₂ sorption isotherm and X-ray diffraction (XRD). The results show that the size and pore characteristics of carbon microsphere obviously depend on stirring speed and concentration of surfactant in the emulsion polymerization process. The resultant CA microspheres are amorphous carbon structure with the size ranging from about 2 to 50 μm by changing the stirring speed. CA microspheres with S_BET of 414-603 m² g^− 1 and V_meso of 0.028-0.432 cm³ g^− 1 are synthesized using different SPAN80 concentrations. The results of cyclic voltammetry indicate that the CA microspheres prepared at a stirring speed of 480 rpm and at V_s/V_h = 0.01 have ideal supercapacitive behavior in 6 M KOH electrolyte, the maximum specific capacitance of the electrode reaches 180 F g^− 1.     

Structural and optical property studies of CdSe crystalline nanorods synthesized by a solvothermal method

CdSe nanorods are synthesized via a simple solvothermal method at a moderate temperature of 180 °C. The influences of introducing hydrazine hydrate (N₂H₄·H₂O) as the reducing agent, and ammonia (NH₃·H₂O) as the complexing agent and also the reaction temperature, on the morphology and size of the obtained CdSe nanorods are investigated and reported. CdSe nanorods with a mean diameter and length of 25 and 82 nm, respectively, are synthesized and the problem of handling the stacking faults present in the long CdSe nanorods is analyzed. The use of increased quantity of hydrazine hydrate and also prolonged reaction time is found to reduce the stacking faults on the synthesized nanorods. The morphology, phase and the optical properties of CdSe nanoparticles are studied using powder X-ray diffraction, TEM and high-resolution transmission electron microscope (HRTEM), UV–visible absorption spectroscopy and photoluminescence (PL) spectroscopy. The low-resolution TEM images confirm the formation of CdSe nanorods, and also the agglomeration of nanoparticles and the presence of few spherical nanoparticles. The strong PL intensity from the CdSe nanorod at 702 nm confirms a blue shift of 14 nm, when compared with the bulk wurtzite CdSe.     

Synthesis and characterization of ilmenite NiTiO3 and CoTiO3 prepared by a modified Pechini method

Powders of ilmenite structure NiTiO₃ and CoTiO₃ were prepared by a simple method based on the modified Pechini process. The raw compounds and citric acid (CA) were mixed in ethanol (EA) with the molar ratio Ni(Co)/Ti/CA/EA = 1/1/1/7.5. The DTA curve shows exothermic peaks only around 300-350 °C and 600 °C, which correspond to the decomposition of the organic compound and direct crystallization of the ilmenite phase. X-ray diffraction patterns indicated that the ilmenite phase was successfully synthesized as the Ni(Co)-Ti precursor calcined above 600-900 °C for 3 h, and the activation energies of NiTiO₃ and CoTiO₃ were calculated to be about 8.84 and 13.23 kJ/mol. TEM bright field images showed that the grain sizes of powders of NiTiO₃ and CoTiO₃ at 600-900 °C were estimated to be about 10-250 and 20-200 nm depending on the nature of the aggregate. The samples of NiTiO₃ calcined at 600-800 °C have the larger specific surface area of 31.51, 18.78, and 6.01 m²/g, respectively. The UV-Vis diffuse reflectance spectra show the optical band gaps of NiTiO₃ and CoTiO₃ as 3.02 and 2.43 eV.     

Hydrothermal synthesis of organic hybrid BaTiO3 nanoparticles using a supercritical continuous flow reaction system

Barium titanate (BaTiO₃: BT) nanoparticles were synthesized by the hydrothermal method in the presence of dispersants using a continuous supercritical flow reaction system. The reactants of TiO₂ sol/Ba(NO₃)₂ mixed solution and KOH solution were used as starting materials and that was heated quickly up to 400 °C under the pressure of 30 MPa for 8 ms as reaction time. The dispersant solution such as polyacrylic acid (PAA) and polyoxyethylene(20) sorbitan monooleate (Tween 80) was injected in the cooling process after the reaction. The crystal phase of the obtained particles was identified as perovskite cubic BaTiO₃ by X-ray diffractometry (XRD) and Raman spectroscopy. Raman spectra and thermogravimetric data revealed that PAA and Tween 80 fabricated hybrid BT nanoparicles. Primarily particle size of the BaTiO₃ nanoparticle was determined by means of BET surface area, as small as less than 10 nm irrespective of dispersants. In contrast, dispersed particle size in solution measured by dynamic light scattering (DLS) technique decreased from 282 nm to less than 100 nm depending on the dispersant. Aggregation of BaTiO₃ nanoparticles might be depressed in the presence of dispersants, especially PAA is the most effective among the dispersants examined.     

Growth of polar axis oriented tetragonal Pb(Zr,Ti)O3 films on CaF2 substrates with transparent (La0.07Sr0.93)SnO3

Epitaxial (La_0.07Sr_0.93)SnO₃ [LSSO] films were deposited on CaF₂ substrates by pulse laser deposition. The (1 0 0)_c orientation of LSSO films was observed only on (1 1 0)CaF₂, whereas (1 1 0)_c orientation was found on (1 1 1)CaF₂ and (1 0 0)CaF₂. (0 0 1) polar axis oriented tetragonal Pb(Zr_0.35Ti_0.65)O₃ films were grown on the fabricated (1 0 0)_cLSSO∥(1 1 0)CaF₂ by pulsed metal organic chemical vapor deposition. The (0 0 1)Pb(Zr_0.35Ti_0.65)O₃∥(1 0 0)cLSSO∥(1 1 0)CaF₂ stack structure exhibited about 70% transparency with an adsorption edge of approximately 330 nm.     

Synthesis of ORMOSIL silica/rhodamine 6G: Powders and compacts

The sol-gel method was used to prepare a silica matrix with rhodamine 6G. This dye was chemically bonded to silica matrix by grafting reactions, obtaining ORMOSIL/R6G powder, at two different concentrations, 0.03 mmol of dye/g silica and 0.009 mmol of dye/g silica, called ORMOSIL1 and ORMOSIL2, respectively. Fluorescent compacts were also obtained, through the high-pressure processing of these powders, at 7.7 GPa and room temperature. The microstructure, chemical composition and thermal stability of the powders and compacts were comparatively studied, by N₂ adsorption/desorption isotherms, FTIR spectroscopy, thermogravimetric analyses (TGA) and elemental analyses for carbon, hydrogen, and nitrogen (CHN). The optical behavior was studied by fluorescence spectroscopy. The ORMOSIL1 compacts were completely opaque showing that the compaction was not effective, due to the high organic grade incorporated into the starting ORMOSIL1 powder. The ORMOSIL2 compacts were transparent showing an effective compaction, which are in agreement to the great surface area and porosity reduction. Additionally, it was observed in TGA results, the retention of the organics in these samples up to temperatures near 300 °C. The fluorescence emission showed that the dye was dispersed in molecular level in all samples.     

Characterization of nanocluster formation in Cu-implanted silica: Influence of the annealing atmosphere and the ion fluence

High-purity silica plates were implanted with 2 MeV Cu⁺ ions at various ion fluences: 0.7 × 10¹⁶, 3 × 10¹⁶ and 6 × 10¹⁶ ions/cm². After implantation, thermal treatments were performed at 400 °C and 900 °C in either an oxidizing (air) or a reducing (50% H₂ + 50% N₂) atmosphere for 1 h. All the samples were studied by electron paramagnetic resonance, X-ray photoelectron spectroscopy, high-resolution transmission electron microscopy (HRTEM), Rutherford backscattering spectrometry and optical absorption. The advantages of the reducing atmosphere (RA) over the oxidizing atmosphere (OA) are clearly observed. When annealed in a RA, the surface plasmon resonance is more intense and a narrower size distribution of the Cu nanoparticles is obtained. The existence of CuO nanoparticles was confirmed by HRTEM, and while both annealing atmospheres favor the formation of CuO nanoparticles, this process is strengthened when the sample is annealed in an OA.     

Low-temperature deposition of crystalline silicon nitride nanoparticles by hot-wire chemical vapor deposition

The nanocrystalline alpha silicon nitride (α-Si₃N₄) was deposited on a silicon substrate by hot-wire chemical vapor deposition at the substrate temperature of 700 °C under 4 and 40 Torr at the wire temperatures of 1430 and 1730 °C, with a gas mixture of SiH₄ and NH₃. The size and density of crystalline nanoparticles on the substrate increased with increasing wire temperature. With increasing reactor pressure, the crystallinity of α-Si₃N₄ nanoparticles increased, but the deposition rate decreased.     

Development of optical nonlinearity, high dielectric constant and ferromagnetic behavior in a silicate glass nanocomposite by suitable heat treatment

We have explored the development of multifunctionalities viz, optical nonlinearity, high dielectric constant and ferromagnetic behavior in a nanostructured silica based glass of 14.0Na₂O, 26.0BaO, 26.0TiO₂, 16.0B₂O₃, 17.0SiO₂, 1.0NiO (mol%) composition. A heat treatment at 863 K for 4 h led to nonlinear refractive index and absorption coefficients at wavelength 800 nm of 0.11 × 10⁻¹⁹ m²/W and 1.15 × 10⁻³ cm/GW, respectively. A heat treatment at 1073 K for 2 h followed by 1113 K for 3 h increased the dielectric constant from 11 to 50, apparently due to the formation of nanocrystals of BaTiO₃ within the glass medium. Glass samples reduced at 923 K for 1 h exhibited ferromagnetic behavior due to the presence of nickel nanoparticles.     

Synthesis,characterization and growing mechanism of monodisperse Fe3O4 microspheres

Monodisperse Fe₃O₄ microspheres assembled by a number of nanosize tetrahedron subunits have been selectively synthesized through the hydrothermal process. The synthesized Fe₃O₄ microspheres have good dispersibility. The subunits made up of microspheres were uniform in size and like-tetrahedron in shape. The average diameter of each Fe₃O₄ microsphere is about 50–55 μm. The length of each edge of tetrahedron is about 100 nm. A series of experiments had been carried out to investigate the effect of reductant, precipitator and reaction time on the formation of Fe₃O₄ microsphere and tetrahedron subunits. The results show that ascorbic acid as reductant and urea as precipitator supplied a relatively steady environment during the synthesis process and led to the formations of Fe₃O₄ tetrahedron subunit and monodisperse Fe₃O₄ microspheres. As the reaction time increased from 3 to 24 h, the Fe₃O₄ microspheres tended towards dispersion and becoming large in size from 10–20 to 50–55 μm, and the subunits formed Fe₃O₄ microspheres that varied from spheroid to tetrahedron and from a small nanoparticle (20–30 nm) to a large one (90–110 nm). A reasonable explanation for the formations of the Fe₃O₄ microsphere and the tetrahedron subunit was proposed through Ostwald ripening and the attachment growth mechanism, respectively.     

Variation of luminescence properties of Na2O-CaO-SiO2: Nd glass with crystallinity

The optical absorption and emission intensities of Nd³⁺-doped transparent glass-ceramics with high crystallinity in Na₂O-CaO-SiO₂ (NSC) system were studied. The transmittance of NCS decreases with increasing degree of crystallinity, however it still remains 65.5% at λ = 710 nm when the crystallization is almost completed. Judd-Ofelt theory is performed to evaluate the radiative transition probability as well as quality factor, branching ratio and emission cross section. The maximum values of Ω₂ and emission cross section (⁴F_3/2 → ⁴I_11/2) of NCS are obtained after nucleating at 630 °C for 10 h. The quality factor increases with increasing crystallinity, while branching ratio for ⁴F_3/2 → ⁴I_11/2 is opposite. The results show that transparent glass-ceramic with high crystallinity is a potential laser host for 1.06 μm emission.     

Synthesis,characterization and application of magnetic-zirconia nanocomposites

In the present study, a magnetic-zirconia nanocomposite was successfully synthesized by a single-step co-precipitation method. The as-prepared nanocomposite was characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, powder X-ray diffraction, and nitrogen sorption measurements. The ultimate material was found to be Fe₃O₄–ZrO₂ nanoparticles with average diameter of 80 nm, high surface area up to 166 m²/g, and strong magnetic property. The application of this new nanocomposite was herein demonstrated by the adsorption of ethyl methylphosphonic acid, a degradation product of nerve agent in water, followed by mass spectrometry detection. Excellent adsorption could be observed, indicating the as-synthesized material was effective to remove phosphonic acid compound from water. Apart from adsorption, the Fe₃O₄–ZrO₂ nanocomposite is promising in various applications such as catalysis and bioseparation.     

Size-controlled synthesis of LaAlO3 by reverse micelle method: Investigation of the effect of water-to-surfactant ratio on the particle size

Lanthanum monoaluminate (LaAlO₃) nanoparticles have been synthesized using microreactors made of poly(oxyethylene) nonylphenyl ether (Igepal CO-520)/water/cyclohexane microemulsions. The control of particle size was achieved by varying the water-to-surfactant molar ratio. The synthesized and calcined powders were characterized by thermogravimetry–differential thermal analysis (TGA-DTA), X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FTIR). Differential thermal analysis showed that LaAlO₃ phase transformation decreases with increase in water/surfactant (R) value. Pure LaAlO₃ phase was synthesized by annealing at 800 °C for 2 h in air directly from amorphous precursors, without formation of intermediate phase. The average particle size was found to increase with increase in water-to-surfactant ratio (R). FTIR analysis was carried to monitor the elimination of residual oil and surfactant phases from the microemulsion-derived precursor and calcined powder.     

Surfactant effects on the particle size of iron (III) oxides formed by sol-gel synthesis

In this work, we probed the effects of a common surfactant, sodium dodecylbenzene sulfonate (NaDDBS), on the particle size of iron (III) oxides formed via a modified sol-gel synthesis. The goal was to create tunable nanosized particles via a method that combines the efficiency and advantages of the sol-gel process, but inhibits the formation of a gel. Two different metal salt precursors were used, ferric nitrate nonahydrate, Fe(NO₃)₃ · 9H₂O, and ferric chlorate hexahydrate, FeCl₃ · 6H₂O. The particle size of the dried gel was 4.5 nm for Fe(NO₃)₃ · 9H₂O and 3.6 nm for FeCl₃ · 6H₂O. In the presence of the surfactant FeCl₃ · 6H₂O formed a gel and Fe(NO₃)₃ · 9H₂O was unable to gel, but the new particle sizes were 4.9 nm and 3.2 nm, respectively. The addition of the surfactant in the later stages of the process afforded the stabilization of independent nanoparticles of the same size as those obtained in the systems that gelled.     

Preparation of Sb2S3 nanomaterials with different morphologies via a refluxing approach

Single-crystalline antimony trisulfide (Sb₂S₃) nanomaterials with flower-like and rod-like morphologies were successfully synthesized under refluxing conditions by the reaction of antimony trichloride (SbCl₃) and thiourea with PEG400 and OP-10 as the surfactants. X-ray diffraction (XRD) indicates that the obtained sample is orthorhombic-phase Sb₂S₃ with calculated lattice parameters a=1.124 nm, b=1.134 nm and c=0.382 nm. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images show that the flower-like Sb₂S₃ is 9–10 μm in size, which is composed of thin leaves with thickness of 0.05–0.2 μm, width of 0.8–2.2 μm and length of 2.5–3 μm, and the rod-like Sb₂S₃ is 45–360 nm in diameter and 0.7–4 μm in length, respectively. UV–Vis analysis indicates that the band gap of Sb₂S₃ nanorods is 1.52 eV, suitable for photovoltaic conversion. A possible mechanism of formation was proposed. The effects of reaction time and surfactants on the growth of nanomaterials with different morphologies were also investigated.     

Structural properties of the tungsten-lead-borate glasses before and after laser irradiation

Glasses in the xWO₃·(100 − x)[3B₂O₃·PbO] system, where 0 ≤ x ≤ 40 mol%, are obtained by conventional melting-quenching method and characterized using X-ray diffraction, FTIR spectroscopy and DFT calculations. These tungsten-lead-borate systems exhibit a photochromic effect which can be induced through laser exposures (λ = 633 nm) directly on the bulk sample. Structural investigations show that the photosensitive effect are due to a reduction of W^+ 6 to W^+ 5 and/or W^+ 4 promoted by the oxidation of Pb^+ 4 and some structural changes of the borate network. DFT calculations show higher thermodynamic stability of the [W₂O₇] and [WO₄] polyhedrons comparative with the [WO₆] polyhedron.     

One-step fabrication of Fe2O3/Ag core-shell composite nanoparticles at low temperature

The Fe₂O₃/Ag core-shell composite nanoparticles were successfully prepared via a simple method at low temperature. X-ray diffraction data revealed the formation of core-shell composite nanoparticles, with Fe₂O₃ as the core and silver as the shell. The results from the transmission electron microscopy and scan electron microscopy further indicated that the composite nanoparticles were spherical with a core diameter and shell thickness of 26.0 nm and 13.5 nm, respectively. Magnetic measurements showed that the composite nanoparticles exhibited a typical ferromagnetic behavior, a specific saturation magnetization of 0.95 emu/g and an intrinsic coercivity of 104.0 Oe at room temperature. For a standard two-probe analysis at room temperature, the composite nanoparticles showed a typical conductive behavior and its conductivity was about 3.41 S/m. Moreover, this present synthesis method of Fe₂O₃/Ag core-shell composite nanoparticles shows an easy processing and does not need high-temperature calcining to attain the final product, which can be applied in a variety of areas, including catalysis, medicine, photonics, and new functional device assemblies.     

Structural, thermal and electrical properties of PVA-LiCF3SO3 polymer electrolyte

The development of polymeric systems with high ionic conductivity is one of the main objectives in Li rechargeable battery. In the present study, the different composition of PVA-LiCF₃SO₃ polymer electrolyte has been prepared by solution cast technique using DMSO as solvent. The FTIR study confirms the polymer-salt complex formation. The amorphous nature of the polymer has been confirmed by XRD analysis. DSC measurements show decrease in T_g with increasing salt concentration. The temperature dependent conductivity obeys Arrhenius relationship. The maximum conductivity has been observed in the order of 7 × 10^− 4 S cm^− 1 for 25 mol% of LiCF₃SO₃. The activation energy has been found to be 0.16 eV. The two peaks have been observed in the dielectric loss spectrum which shows two types of relaxation α and β.     

Optical and structural characterization of nickel selenide nanoparticles synthesized by simple methods

A series of nickel selenide (NiSe₂, NiSe and Ni₃Se₄) nanoparticles have been synthesized by three different methods, i.e. the single-source precursor (method 1), the thermolysis of trioctylphosphine selenide (TOPSe) and nickel chloride in hexadecylamine (method 2) as well as the reaction of nickel chloride and selenium using sodium borohydride as a reducing agent in methanol and in water (method 3). The optical properties of nickel selenide synthesized from all the methods showed good nanometric characteristics with an observed blue-shift in absorption band-edge from bulk nickel selenide. The structural characteristics varied with the methods employed, with method 1 producing 10 nm spherical NiSe₂ particles, method 2 star-shaped NiSe particles, while method 3 produced hexagonal NiSe nanoparticles in methanol and rod-shaped Ni₃Se₄ particles in water.     

Morphology control of MSU-1 silica particles

Mesoporous silica, MSU-1 with spherical morphology was prepared using TEOS (tetraethylorthosilicate) as a silica source in the presence of an alkyl polyethylene oxide surfactant via the novel two-step process proposed by Prouzet’s group: hydrolysis of TEOS conducted in highly acidic condition at room temperature followed by condensation promoted by fluoride salt addition at 35 °C. The particles produced were characterized by XRD, SEM, and N₂ adsorption/desorption isotherm. Static condensation period was found to be essential to have spherical morphology. Growth of spherical particles and evolution of porosity were studied as a function of time, temperature, NaF/TEOS, and TEOS/surfactant ratio. The MSU-1 particles prepared under different synthesis conditions were briefly tested for chromatographic separation of selected organic molecules, which demonstrates the governing influence of the pore size in MSU-1 on retention time.