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Mixed structure Zn(S,O) nanoparticles: synthesis and characterization

Abstract

In the present work, mixed structure Zn(S,O) nanoparticles have been synthesized using solution based chemical coprecipitation technique. Two different zinc sources (Zn(CH3COO)2·2H2O and ZnSO4·7H2O) and one sulfur source (CSNH2NH2) have been used as primary chemical precursors for the synthesis of the nanoparticles in the presence and absence of a capping agent (EDTA). The structural, morphological, compositional and optical properties of the nanoparticles have been analyzed using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), Fourier transmission infra-red (FT-IR) and UV-Visible (UV-Vis) spectroscopy. XRD revealed the formation of mixed phases of c-ZnS, h-ZnS and h-ZnO in the synthesized nanoparticles. The surface morphology was analyzed from SEM micrographs which showed noticeable changes due to the effect of EDTA. EDX analysis confirmed the presence of zinc, sulfur and oxygen in Zn(S,O) nanoparticles. FT-IR spectra identified the presence of characteristic absorption peaks of ZnS and ZnO along with other functional group elements. The optical band gap values were found to vary from 4.16 eV to 4.40 eV for Zn(S,O) nanoparticles which are higher in comparison to the band gap values of bulk ZnS and ZnO. These higher band gap values may be attributed to the mixed structure of Zn(S,O) nanoparticles.

Open access
Problems of Pad Welding Structural Steels with Martensitic Filler Metal

Abstract

There is a problem in obtaining a suitable impact strength of the padding weld after cladding with a martensitic filler metal. Too low annealing temperature below 580°C and the excessive annealing temperature above 650°C do not provide adequate impact strength of the padding weld. A heat treatment technology for mixed joints has been developed based on the results of the microscopic observations, X-ray diffraction measurements and transmission electron microscope examination. The problem was identified and a special technology of heat treatment for the dissimilar joint was elaborated. This technology provides a high impact resistance of the padding weld and an appropriate properties of the base material.

Open access
Selective crystallization of gamma glycine for NLO applications using magnesium sulfate (MgSO4) as an additive

Abstract

Crystallization of γ-glycine in the presence of selected concentration (9 g/mL) of tailor-made additive magnesium sulfate heptahydrate salt (MgSO4·7H2O) has been studied at ambient temperature by adopting slow solvent evaporation procedure. The morphological modifications of glycine crystals grown from pure aqueous solutions of glycine and from glycine solutions containing magnesium species in the amount of 0.1 g/mL to 16 g/mL have been investigated thoroughly. The crystalline nature and phase identification of the crystalline material were confirmed by X-ray powder diffraction and SXRD studies. NMR studies revealed the information about the molecular conformation in solution, phase changes, functional groups and chemical environment. FT-IR spectra revealed distinct difference between α and γ-glycine polymorphs in the region around 880 cm−1 to 930 cm−1. The grown γ-glycine crystal had a lower cut-off value at 200 nm and the bandgap value evaluated from the Tauc plot was found to be 5.83 eV. The marked differences between α and γ-polymorphs of glycine were also revealed by DSC thermograms. The mechanical strength of the γ-glycine crystal was studied with the help of Vickers microhardness instrument. Kurtz-powder NLO study proved the generation of second harmonics (i.e. green light emission) in the grown γ-glycine crystal and its efficiency was calculated as 1.44 times better than that of the reference material potassium dihydrogen phosphate.

Open access
Structural and thermal properties of Zn-containing magnesium aluminate spinels obtained by wet chemical method

Abstract

In the present study, the dopant effect of Zn on the crystal structure, thermal properties and morphology of magnesium aluminate (MgAl2O4) spinel (MAS) structure was investigated. A pure and two Zn-containing MASs (e.g. MgAl1.93Zn0.07O4 and MgAl1.86Zn0.14O4) were synthesized for this purpose via a wet chemical method, and the as-prepared samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, differential thermal analysis (DTA), thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy techniques. It was found that the crystal structure, thermal properties and morphology of the MAS system change with the increase in the amount of Zn. MgO phase formation was observed. The values of the lattice parameter, unit cell volume and crystallite size increased, and the crystallinity percentage decreased. The morphology was also affected by adding of Zn.

Open access
Structural optical and magnetic properties of transition metal doped ZnO magnetic nanoparticles synthesized by sol-gel auto-combustion method

Abstract

Transition metals, such as chromium (Cr) and manganese (Mn) doped zinc oxide (ZnO) magnetic nanoparticles, were synthesized via sole gel auto-combustion method. The prepared magnetic (Zn1−(x+y)MnxCryO, where x, y = 0, 0.02, 0.075) nanoparticles were calcined in an oven at 6000 °C for 2 hours. The morphologies of the nanoparticles were investigated using different techniques. X-ray diffraction (XRD) analysis revealed that the hexagonal wurtzite structure of the synthesized nanoparticles was unaffected by doping concentration. The crystallite size measured by Scherrer formula was in the range of 32 nm to 38 nm at different doping concentrations. Nanosized particles with well-defined boundaries were observed using a field emission scanning electron microscopy (FE-SEM). Fourier transform infrared (FT-IR) spectra showed a wide absorption band around 1589 cm−1 in all the samples, corresponding to the stretching vibration of zinc and oxygen Zn–O bond. A blue shift in optical band gaps from 3.20 eV for ZnO to 3.08 eV for Zn0.85Mn0.075Cr0.075O nanoparticles was observed in diffuse reflectance spectra, which was attributed to the sp-d exchange interactions. The field-dependent magnetization M-H loops were measured using vibrating sample magnetometer (VSM). The VSM results revealed diamagnetic behavior of the ZnO nanoparticles which changed into ferromagnetic, depending on the doping concentration and particle size. The compositions of Zn, Cr, Mn and O in the prepared samples were confirmed by using the energy dispersive X-ray spectroscopy (EDX). Our results provided an interesting route to improve magnetic properties of ZnO nanoparticles, which may get significant attention for the fabrication of magnetic semiconductors.

Open access
Structural, optical, thermal, dielectric and mechanical studies of a new organic NLO material: L-isoleucinium p-toluenesulfonate monohydrate (LIPT)

Abstract

In the present work, a new organic second order NLO material: L-isoleucinium p-toluenesulfonate monohydrate (LIPT) is synthesized and reported for the first time. The LIPT is crystallized in a non-centrosymmetric monoclinic space group P21. Structural and hydrogen bond nature of the compound is analyzed using single crystal X-ray diffraction studies. The crystal exhibits very good optical properties such as wide optical transparency in the region of 210 nm to 1100 nm and the ultraviolet wavelength emission (λ = 283 nm). The second harmonic generation efficiency is found to be 1.7 times the standard KDP. Good thermal, mechanical properties and low dielectric constant at high frequency range show that the material may be a potential candidate for optoelectronic applications.

Open access
Studies on Cu2SnS3 quantum dots for O-band wavelength detection

Abstract

In this communication, we report on Cu2SnS3 quantum dots synthesized by the solvothermal process using different solvents. The optical properties of the quantum dots are analyzed by UV-Vis-NIR and photoluminescence spectroscopy. The results suggest that Cu2SnS3 material has tunable energy bandgap and appropriate wavelength for fabrication of light emitting diodes and laser diodes as sources for fiber optic communication. They exhibit wide absorption in the near infrared range. Further morphological studies with the use of atomic force microscope confirm the surface topography and the existence of quantum dots. The observed characteristics prove the efficiency of Cu2SnS3 quantum dots for O-band wavelength detection used in fiber optic communication and solar cell applications.

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Synthesis and optical properties of CdSe/CdS core/shell nanocrystals

Abstract

This paper attempts to describe an effective method for producing a composite of quantum dots consisting of CdSe (core) with CdS (shell). This nanoparticles composite was synthesized from modified organometallic precursors. The sizes of the nanoparticles were estimated from X-ray diffraction data using Debye-Scherer formula and compared with high resolution electron microscopy (HRTEM) and optical spectra. The shape of CdSe/CdS NPs is nearly spherical and revels that the CdS shell with the thickness ~0.6 nm almost fully covers the CdSe core (higher contrast). Using UV-Vis spectroscopy, a systematic red shift in the absorption and emission spectra was observed after the deposition of CdS which confirms the shell growth over the CdSe core. In the CdSe/CdS core/shell structure, the holes are confined to the core, while the electrons are delocalized as a result of similar electron affinities of the core and the shell. The increased time of synthesis resulted in shell thickness increase. The observed properties of prepared CdSe/CdS QDs demonstrate the capability of the nanocomposite for using in the optoelectronics and photonics devices.

Open access
Synthesis, growth and characterization of NaAl(SO4)·H2O triangular prism single crystal for inorganic NLO application

Abstract

An inorganic coordination complex of single crystal containing sodium and aluminum (SA) was grown at room temperature by slow evaporation technique. The crystal was characterized using single crystal X-ray diffraction (XRD), FT-IR, UV-Vis, SHG, SEM, EDX and TG/DTA analyses. The size of the grown crystal was around 17 mm × 15 mm × 5 mm. Both optical and SEM photographs confirmed that the crystal is transparent with smooth surface. The XRD data showed that the crystal belongs to the BCC crystal structure. The crystal shows excellent transparency in the entire region of visible light (cut-off value is 339 cm−1). The dielectric constant as well as dielectric loss of the sample was calculated by varying frequencies at different temperatures and the presence of low dielectric loss proved that this crystal can be used for the NLO application.

Open access
Wetting properties of titanium oxides, oxynitrides and nitrides obtained by DC and pulsed magnetron sputtering and cathodic arc evaporation

Abstract

Thin films of titanium oxides, titanium oxynitrides and titanium nitrides were deposited on glass substrates by the methods of direct current (DC) and pulsed magnetron sputtering and cathodic arc evaporation. Phase analysis of the deposited films by X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FT-IR) showed the presence of phases with various Ti oxidative states, which indicated a high concentration of oxygen vacancies. The films morphology was investigated by scanning electron microscopy (SEM). Investigations of the films wettability, either with water or ethylene glycol, showed that it depends directly on the concentration of oxygen vacancies. The wettability mechanism was particularly discussed.

Open access