Fabrication and characterization of silver/titanium dioxide composite nanoparticles in ethylene glycol with alkaline solution through sonochemical process

This paper aims to study fabrication and characterization of silver/titanium oxide composite nanoparticle through sonochemical process in the presence of ethylene glycol with alkaline solution. By using ultrasonic irradiation of a mixture of silver nitrate, the dispersed TiO₂ nanoparticle in ethylene glycol associated with aqueous solution of sodium oxide yields Ag/TiO₂ composite nanoparticle with shell/core-type geometry. The powder X-ray diffraction (XRD) of the Ag/TiO₂ composites showed additional diffraction peaks corresponding to the face-centered cubic (fcc) structure of silver crystallization phase, apart from the signals from the cores of TiO₂. Transmission electron microscopy (TEM) images of Ag/TiO₂ composites, which average particle size is roughly 80 nm, reveal that the titanium oxide coated by Ag nanoparticle with a grain size of about 2–5 nm. Additionally, the formation of silver nanoparticles on TiO₂ was monitored by ultraviolet visible light spectrophotometer (UV–Vis). As measured the optical absorption spectra of as-synthesized Ag nanoparticle varying with time, the mechanism of surface formatting silver shell on the cores of TiO₂ could be explored by autocatalytic reaction; the conversion of Ag particle from silver ion is 98% for the reaction time of 1000 s; and the activity energy of synthesizing Ag nanoparticles on TiO₂ is 40 kJ/mol at temperature ranging from 5 to 25 °C. Hopefully, this preliminary investigation could be used for mass production of composite nanoparticles assisted by ultrasonic chemistry in the future.     

A new and straightforward synthesis route for preparing Cds quantum Dots

In this work, highly stable, soluble and luminescent CdS quantum dots (QDots) with a narrow size distribution were synthesized in ethylene glycol using the polyol process and the solvothermal technique. In this case instead of using a conventional highly toxic sulfur source like H₂S, we use elemental sulfur dissolved in ethylene glycol to perform the reaction. When the solvent reaches its boiling point inside the autoclave, sulfur is reduced to S^?2 and reacts with Cd⁺² ions to form CdS nanocrystals. Analysis of the spectroscopic and TEM measurements showed that 3 nm monodispersed CdS QDots were synthesized and exhibited high photoluminescence (PL) in the blue green region of the spectra when excited with 355 nm.     

Growth-morphology-luminescence correlation in ZnO-containing nanostructures synthesized in different media

Zinc hydroxide particles were prepared by a two-step process employing zinc nitrate hexahydrate, urea, ethylene glycol, water and p-toluene-sulfonic acid monohydrate (p-TSA). We used different concentrations of the reactants as well as different volume ratios of the solvents. ZnO particles were obtained by thermal treatment of the reaction products at two different temperatures: 350 °C and 500 °C. The samples were characterized by scanning field emission electron microscopy (SEM), X-ray diffraction (XRD) spectroscopy, BET analysis, thermogravimetry (TG) analysis and photoluminescence (PL) spectroscopy. It was found that after the thermal treatment particles become smaller, with the p-TSA concentration strongly affecting the morphology of the particles. Luminescence properties of the samples probed by PL at 8 K and room temperature exhibited a remarkable correlation with specimens′ nanomorphology. Luminescent features at ～2.0–2.2 eV, ～2.4–2.5 eV, ～2.65 eV, ～2.9 eV, ～3.0–3.1 eV and ～3.3 eV were observed in most specimens, although their relative intensity and temperature dependence were specific to an individual group of samples vis-à-vis their growth history and morphology.     

Study of Schottky contact between Au and NiO nanowire by conductive atomic force microscopy (C-AFM): The case of surface states

In this work, NiO nanowires have been synthesized by a hydrothermal reaction of NiCl₂ with Na₂C₂O₄ in the presence of ethylene glycol at 180 °C for 12 h, then calcinated at 400 °C for 2 h. The NiO nanowires were analyzed by means of scanning electron microscope (SEM), atomic force microscope (AFM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The resulting current–voltage (I–V) characteristics of the NiO nanowires exhibited a clear rectifying behavior. This rectify behavior was attributed to the formation of a Schottky contact between Au coated atomic force microscopy (AFM) tip and NiO nanowires (nano-M/SC) which was dominated by the surface states in NiO itself. Photo-assisted conductive AFM (PC-AFM) was used to demonstrate how the I–V characteristics are influenced by the surface states. Our I–V results also showed that the nano-M/SCs had a good photoelectric switching effect at reverse bias.     

Synthesis,characterization and mechanical properties of nylon–silver composite nanofibers prepared by electrospinning

Silver (Ag) nanoparticles (∼3 nm) were synthesized using silver nitrate as the starting precursor, ethylene glycol as solvent and poly (N-vinylpyrrolidone) (PVP) introduced as a capping agent. These nano-Ag particles were reinforced in nylon matrix by electrospinning of nylon-6/Ag solution in 2,2,2-trifluoroethanol and composite nanofibrous membranes were synthesized. The effects of solution concentration and relative humidity (RH) on the resultant fibrous membranes were studied. Scanning electron microscopy and Transmission electron microscopy was used to study the size and morphology of the fibers. It was observed that concentration and RH could be used to modulate the fiber diameter. Tensile test was used to evaluate the mechanical property of these electrospun composite membranes. The composite membranes showed higher strength (approx. 2–3 times increase in strength) compare to as synthesized nylon fibers.     

Luminescence and physical properties of copper doped CdO derived nanostructures

In this paper, we studied the photoluminescence (PL), the morphological, electrical and optical properties of pure and copper-doped cadmium oxide. CdO films were grown by a facile sol–gel spin coating process at 1200 rpm, and doped with copper at 2 and 3%. A (1 1 1)-oriented cubic structure with a lattice parameter of a=4.69 Å was confirmed by X-ray diffraction. Copper was shown to improve the optical transmittance in the short wavelength range of the visible spectrum. The optical band gap of CdO ranged between 2.49 and 2.62 eV as a result of Cu content. At room temperature, resistance fell drastically with Cu doping levels. AFM analysis of samples exhibited nano-mounts and nanowires. Finally, PL results showed a strong blue–violet emission peak at 2.80 eV.     

Photoluminescence study on amino functionalized dysprosium oxide–zinc oxide composite bifunctional nanoparticles

An organic dispersion of 9–15 nm size stable dysprosium oxide incorporated zinc oxide nanocomposites exhibiting luminescence in the visible region has been synthesised by a wet chemical precipitation technique at room temperature. Tetraethoxysilane TEOS [(C₂H₅O)₄Si], (3-aminopropyl) trimethoxysilane (APTS) and a 1:1 mixture of TEOS–APTS have been used as capping agents to control the particle size as well as to achieve uniform dispersion of composite nanoparticles in methanol medium. X-ray diffractometer (XRD) analysis reveals the formation phase of amino-functionalised colloidal dysprosium oxide incorporated ZnO composite nanoparticles to be of zincite structure. The Transmission Electron Microscopy (TEM) images show that the particles are spheroids in shape, having average crystalline sizes ranging from 9 to 15 nm. The photoluminescence (PL) observed in these composites has been attributed to the presence of near band edge excitonic emission and existence of defect centres. The time correlated single photon counting studies of the composite nanoparticles exhibited three decay pathways. The enhanced PL emission intensity of solid state fluorescence spectra of samples is attributed to the absence of vibrational relaxation process.     

Photoluminescence characterization of beryllium-implanted 6H–silicon carbide

Beryllium has been implanted into both n- and p-type 6H–SiC with post-implantation annealing at 1600 °C. Photoluminescence (PL) measurements have been performed, and PL lines at 420.5, 431 nm, and a broad band at around 505 nm have been observed. The line at 420.5 nm is attributed to an intrinsic defect D_II-center induced by beryllium implantation. The effects of excitation intensity and temperature during the PL experiments are investigated. Based on the excitation laser dependence PL result, the new doublet lines at around 431 nm are thought to be associated with beryllium related bound excitons. The broad band corresponding to the green luminescence at room temperature has been attributed to the recombination of free carriers to beryllium bound levels.     

Nonlinear optical properties of silver colloidal solution by in situ synthesis technique

The silver colloidal solutions were prepared by in situ synthesis technique in the presence of the Polymethyl Methacrylate, which was polymerized by reversible addition-fragmentation transfer. The UV–VIS spectra and transmission electron microscopy had shown the formation of sphere silver nanoparticles with average size of 10 nm. Nonlinear optical properties as a function of silver concentration were studied using Z-scan technique with 13 ns pulse duration at 532 nm. The optical nonlinearity enhancement was observed by increasing the concentration. The third-order nonlinear susceptibility χ⁽³⁾ was measured to 1.045 × 10⁻¹¹ esu when the concentration was 2.13 mg/ml. Besides, the sample was founded to exhibit a shift from saturable absorption to reverse saturable absorption at higher incident laser energy. The reverse saturable absorption was observed to be responsible for the optical limiting characteristics in our experiments.     

Synthesis of LiFePO4 nanoparticles and their electrochemical properties

LiFePO₄ nanoparticles were synthesized via polyol process. The temperature of the solution was rapidly increased up to 320 °C to obtain larger particles and the temperature was maintained for 16 h in a round-bottomed flask attached to a refluxing condenser. The X-ray diffractrion (XRD), pattern was indexed on the basis of orthorhombic olivine structure. The LiFePO₄ compound prepared through polyol process exhibited a high crystallinity. The particles show the various shapes with size ranging from 100 to 300 nm. The initial discharge curve of LiFePO₄ capacity shows 168 mA h/g at the 0.1C rate in the voltage range of 2.5–4 V with well-formed plateau.     

Development of cholesterol biosensor with high sensitivity using dual-enzyme immobilization into the mesoporous silica materials

Mesoporous silica (MPS) materials with different pore diameters were synthesized by a sol–gel method where organic templates such as cationic surfactant (cetyltrimethylammonium bromide) and triblock co-polymer of (poly(ethylene glycol)–poly(propylene glycol)–poly(ethylene glycol) (Pluronic P123, EO₂₀PO₇₀EO₂₀)), were used. MPS surface was organo-functionalized using a silane coupling reagent (ethyl-, phenyl-, or 3-mercaptpropyltriethoxysilane). Dual-enzyme, cholesterol esterase (10.0 nm × 5.4 nm × 11.0 nm) and cholesterol oxidase (6.8 nm × 8.5 nm × 8.8 nm), was immobilized on MPS materials by physical adsorption. Amount of dual-enzyme immobilized on all MPS materials, having a different pore size (2.7, 6.4, 12.4, 14.7, and 22.6 nm), and organo-functionalized MPS was similar (CE: 1.5 mg/mg silica and CO: 0.01 mg/mg silica). High activity of dual-enzyme was obtained by adjacently immobilizing on MPS materials. Its activity on MPS-2 (pore diameter: 6.4 nm) or MPS-5 (pore diameter: 22.6 nm) showed approximately 60% of native activity. Moreover, dual-enzyme immobilized on MPS with highly hydrophobic organo-functional groups (phenyl- or mercaptopropyl-group) exhibited higher activity than that on no-substituted MPS. Relative activity of dual-enzyme immobilized on organo-functionalized MPS-2 increased from 58% to 93%, under the optimum conditions.     

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.     

Preparation of SiC nanowires with fins by chemical vapor deposition

SiC nanowires with fins have been prepared by chemical vapor deposition in a vertical vacuum furnace by using a powder mixture of milled Si and SiO₂ and gaseous CH₄ as the raw materials. The products were characterized by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). These investigations confirm that the nanowires with fins are cubic β-SiC. The diameter of the fins is about 100–120 nm and the diameter of the inner core stems is about 60–70 nm. The formation process of the β-SiC nanowires with fins is analyzed and discussed briefly.     

The origin of yellow band emission and cathodoluminescence of Au-catalyzed wurtzite GaN nanowires

GaN nanowires with large yield are directly synthesized by simply ammoniating the gallium oxide powders in the presence of ammonia gas at 1000 °C, under the assistance of Au nanocatalysts. The microstructure and crystallinity of as-synthesized GaN nanowires are well studied by using high-resolution transmission electron microscope (HRTEM) and some structural defects such as stacking faults are found in the GaN nano-crystal. Cathodoluminescence measurement shows that a strong near-band-edge (NBE) emission band centered at 384 nm and a broad yellow band in the range of 500–800 nm are observed. Finally, the growth mechanism and possible optical emission process of GaN nanowires are discussed.     

Study of size dependent photoluminescence properties of copper doped sodium hexametaphosphate capped ZnS nanoparticles

Copper doped ZnS nanoparticles stabilized by sodium hexametaphosphate (SHMP) have been prepared via the wet chemical method using thiourea and sodium sulphide as chalcogenide sources. The XRD pattern showed that ZnS nanoparticles had zinc blende structure and line broadening suggests the formation of an amorphous compound. Absorption measurements were done for three different concentrations of dopant concentrations. The PL spectrum for the sample synthesized using Na₂S·9H₂O showed a sharp emission peak around 510 nm with full width at half maximum (FWHM)<10 nm. The role of the capping agent and sulphide source on optical properties of as synthesized nanoparticles by steady-state photoluminescence (PL) spectroscopy has been studied.     

Defect related luminescence in Hg0.2Cd0.8Te nano- and micro-crystals grown by the solvothermal method

The photoluminescence (PL) properties of nano- and micro-crystalline Hg_1?xCd_xTe (x≈0.8) grown by the solvothermal method have been studied over the temperature range 10–300 K. The emission spectra of the samples excited with 514.5 nm Ar⁺ laser consist of five prominent bands around 0.56, 0.60, 0.69, 0.78 and 0.92 eV. The entire PL band in this NIR region is attributed to the luminescence from defect centers. The features like temperature independent peak energy and quite sensitive PL intensity, which has a maximum around 50 K is illustrated by the configuration coordinate model. After 50 K, the luminescence shows a thermal quenching behavior that is usually exhibited by amorphous semiconductors, indicating that the defects are related to the compositional disorder.     

Synthesis and application of molecularly imprinted nanoparticles combined ultrasonic assisted for highly selective solid phase extraction trace amount of celecoxib from human plasma samples using design expert (DXB) software

In this work molecular imprinted nanoparticles (MINPs) was synthesized and applied for ultrasonic assisted solid phase extraction of celecoxib (CEL) from human plasma sample following its combination by HPLC–UV. The MINPs were prepared in a non-covalent approach using methacrylic acid as monomer, CEL as template, ethylene glycol dimethacrylate as cross-linker, and 2,2-azobisisobutyronitrile (AIBN) as the initiator of polymerization. pH, volume of rinsing and eluent solvent and amount of sorbent influence on response were investigated using factorial experimental design, while optimum point was achieved and set as 250 mg sorbent, pH 7.0, 1.5 mL washing solvent and 2 mL eluent by analysis of results according to design expert (DX) software. At above specified conditions, CEL in human plasma with complicated matrices with acceptable high recoveries (96%) and RSD% lower than 10% was quantified and estimated.The proposed MISPE-HPLC–UV method has linear responses among peak area and concentrations of CEL in the range of 0.2–2000 μg L⁻¹, with regression coefficient of 0.98. The limit of detection (LOD) and quantification (LOQ) based on three and ten times of the noise of HPLC peaks correspond to blank solution were 0.08 and 0.18 μg L⁻¹, respectively.     

The photoluminescence properties of TiO2-sheathed ZnSe nanowires

ZnSe nanowires have been synthesized by thermal evaporation of ZnSe powders on gold-coated Al₂O₃(0 0 0 1) substrates and then sheathed with TiO₂ by sputtering. Our results show that sheathing Zn nanowires with thin TiO₂ layers can significantly enhance the photoluminescence (PL) emission intensity. XPS analysis results suggest that the PL enhancement is attributed to increases in the concentrations of deep levels such as oxygen and titanium interstitials as well as the density of interface states. The PL emission of ZnSe nanowires is also enhanced by thermal annealing. Annealing in an argon atmosphere is more efficient in enhancing the PL emission than annealing in an oxygen atmosphere.     

Temperature dependent structural and optical properties of tin oxide nanoparticles

Nanocrystalline tin oxide (SnO₂) powders were synthesized through wet chemical route using tin metal as precursor. The morphology and optical properties, as well as the effect of sintering on the structural attributes of SnO₂ particles were analyzed using Transmission electron microscopy (TEM), UV–visible spectrophotometry (UV–vis) and X-ray diffraction (XRD), respectively. The data revealed that the lattice strain plays a significant role in determining the structural properties of sintered nanoparticles. The particle size was found to be 5.8 nm, 19.1 nm and 21.7 nm for samples sintered at 300 °C, 500 °C, and 700 °C, respectively. Also, the band gaps were substantially reduced from 4.1 eV to 3.8 eV with increasing sintering temperatures. The results elucidated that the structural and optical properties of the SnO₂ nanoparticles can be easily modulated by altering sintering temperature during de novo synthesis.     

The preparation and characterization of nanoparticle TiO2/Ti films and their photocatalytic activity

Nanoparticle TiO₂/Ti films were prepared by a sol–gel process using Ti(OBu)₄ as raw material, the as-prepared film samples were also characterized by TG-DTA, XRD, TEM, SEM, XPS, DRS, PL, SPS and EFISPS testing techniques. TiO₂ nanoparticles experienced two processes of phase transition, i.e. amorphous to anatase and anatase to rutile at the calcining temperature range from 450 to 700 °C. TiO₂ nanoparticles calcined at 600 °C had similar composition, structure, morphology and particle size with the internationally commercial P-25 TiO₂ particles. Thus, the conclusion that 600 °C might be the most appropriate calcining temperature during the preparation process of nanoparticle TiO₂/Ti film photocatalysts could be made by considering the main factors such as the properties of TiO₂ nanoparticles, the adhesion of nanoparticle TiO₂ film to Ti substrate, the effects of calcining temperature on Ti substrate and the surface characteristics and morphology of nanoparticle TiO₂/Ti film for the practice view. The Ti element mainly existed on the nanoparticle TiO₂/Ti(3) film calcined at 600 °C as the chemical state of Ti⁴⁺, while O element mainly existed as three kinds of chemical states, i.e. crystal lattice oxygen, hydroxyl oxygen and adsorbed oxygen with increasing band energy. Its photoluminescence (PL) spectra with a peak at about 380 nm could be observed using 260 nm excitation, possibly resulting from the electron transition from the bottom of conduction band to the top of valence band. The PL peak position was nearly the same as the onset of its diffuse reflection spectra (DRS) and surface photovoltage spectroscopy (SPS), demonstrating that the effects of the quantum size on optical property were greater than that of the Coulomb and surface polarization. The PL spectra with two peaks related to the anatase and rutile, respectively, could be observed using the excited wavelength of 310 nm. Weak PL spectra could be observed using the excited wavelength of 450 nm, resulting from surface states. In addition, during the experimental process of the photocatalytic degradation phenol, the photocatalytic activity of nanoparticle TiO₂/Ti film with three layers calcined at 600 °C was the highest.