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Single Step Solid-State Synthesis of Lanthanum Molybdate

Abstract

In this study, LaxMoyOz powders were synthesized by a cost-effective solid-state synthesis method. Four different heating cycles were designed to investigate the effects of synthesis temperature and holding time on lanthanum molybdate (LMO) formation, phase assemblies, particle size and morphology. X-Ray Diffraction (XRD) and scanning electron microscopy (SEM) studies were performed to observe crystal structure and particle morphology of synthesized powders. The results showed that nearly ninety percent β - La2Mo2O9 (43,3 nm crystal size) phase was obtained at 1000 °C for 6 h holding time. Longer holding times at 1000 °C favor more oxygen-rich compounds which cause recrystallization of various new crystalline phases. The grain size of the synthesized powder was increased from 0,2 µm to 1,5 µm with increasing holding time. In summary, it is possible to manufacture LMO powders rich in β - La2Mo2O9 by one - step solid - state synthesis method. The phase assembles and particle size of LMO powders could also be tailored by optimization of heat treatment cycle.

Open access
Structural analysis and dielectric relaxation mechanism of conducting polymer/volcanic basalt rock composites

Abstract

In this work, polypyrrole and polythiophene conducting polymers (CPs) have been synthesized and doped with volcanic basalt rock (VBR) in order to improve their dielectric properties for technological applications. The structure and morphology of the composites with different VBR doping concentrations were characterized by FT-IR and SEM analyses. The best charge storage ability was achieved for maximum VBR doping concentration (50.0 wt.%) for both CPs. Dielectric relaxation types of the composites were determined as non-Debye type due to non-zero absorption coefficient and observation of semicircles whose centers were below Z′ axis at the Nyquist plots. It was also ascertained that VBR doping makes the molecular orientation easier than for non-doped samples and reduced energy requirement of molecular orientation. In addition, AC conductivity was totally masked by DC conductivity for all samples at low frequency.

Open access
Structural and surface analysis of chemical vapor deposited boron doped aluminum nitride thin film on aluminum substrates

Abstract

Chemical vapor deposition (CVD) process was conducted for synthesis of boron (B) doped aluminum nitride (B-AlN) thin films on aluminum (Al) substrates. To prevent melting of the Al substrates, film deposition was carried out at 500 °C using tert-buthylamine (tBuNH2) solution delivered through a bubbler as a nitrogen source instead of ammonia gas (NH3). B-AlN thin films were prepared from three precursors at changing process parameters (gas mixture ratio). X-ray diffraction (XRD) technique and atomic force microscope (AFM) were used to investigate the structural and surface properties of B-AlN thin films on Al substrates. The prepared thin films were polycrystalline and composed of mixed phases {cubic (1 1 1) and hexagonal (1 0 0)} of AlN and BN with different orientations. Intensive AlN peak of high intensity was observed for the film deposited at a flow rate of the total gas mixture of 25 sccm. As the total gas mixture flow decreased from 60 sccm to 25 sccm, the crystallite size of AlN phase increased and the dislocation density decreased. Reduced surface roughness (10.4 nm) was detected by AFM for B-AlN thin film deposited on Al substrate using the lowest flow rate (25 sccm) of the total gas mixture.

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Structural, morphological, optical and diode properties of chemical bath deposited nano-structured CdS thin films using EDTA as a complexing agent

Abstract

CdS thin films with (1 1 1) orientation were prepared by chemical bath deposition technique at 80±5 °C using the reaction between NH4OH, CdCl2 and CS(NH2)2. The influence of annealing temperature varying from 150 °C to 250 °C was studied. X-ray diffraction studies revealed that the films are polycrystalline in nature with cubic structure. Various parameters, such as dislocation density, stress and strain, were also evaluated. SEM analysis indicated uniformly distributed nano-structured spherically shaped grains and net like morphology. Optical transmittance study showed the wide transmittance band and absence of absorption in the entire visible region. I-V characterization of p-Si/n-CdS diode and photoluminescence studies were also carried out for the CdS films.

Open access
Studies on the growth and characterization of L-cysteine hydrogen fluoride single crystal

Abstract

L-cysteine hydrogen fluoride (LCHF) single crystals were grown from aqueous solution. Single crystal X-ray diffraction, FT-IR, UV-Vis-NIR, and TG-DTA were used to test the grown crystals. The specimen dielectric and mechanical behaviors were also studied. Powder X-ray diffraction of the grown crystal was recorded and indexed. The optical properties of the LCHF crystal were determined using UV-Vis spectroscopy. It was found that the optical band gap of LCHF was 4.8 eV. The crystal functional groups were identified using FT-IR. Second harmonic generation (SHG) efficiency of the LCHF was three times higher than that of KDP. The dielectric constant, dielectric loss and AC conductivity were measured at different frequencies and temperatures.

Open access
Synthesis and characterization of binary and ternary nanocomposites based on TiO2, SiO2 and ZnO with PVA based template-free gel combustion method

Abstract

Binary and ternary nanocomposites based on TiO2, SiO2 and ZnO were synthesized by PVA-based template-free gel combustion method. The morphology and the particles sizes of the synthesized samples depended on some parameters including the initial concentrations of metal salts and PVA amount in the sol, solvent composition and solution pH. Effects of these parameters were investigated and optimized by using the Taguchi method. In the experimental design, the Taguchi L25 array was used to investigate six factors at five levels. The samples were characterized by dynamic light scattering (DLS), transmission electron microscopy (TEM), Brunauer-Emmett-Teller (BET) specific surface areas, scanning electron microscopy (SEM). The obtained results showed that the present method can be used to synthesize TiO2/SiO2/ZnO ternary nanocomposite with an effective surface area of 0.3 m2 · g−1 and ZnO/TiO2, TiO2/SiO2, ZnO/SiO2 binary nanocomposites with an effective surface area of 234 m2 · g−1, 6 m2 · g−1 and 0.5 m2 · g−1, respectively. The ZnO/TiO2 nanocomposite which was synthesized under the following experimental conditions: 2.5 wt.% Zn salt, 2.5 wt.% Ti salt, 2.0 wt.% PVA, pH = 1 and ethanol:water ratio 30:70 was selected by the Taguchi method as an optimum sample with the smallest particles (average diameter = 50 nm).

Open access
Synthesis, Characterization and Some Biological Properties of PVA/PVP/PN Hydrogel Nanocomposites: Antibacterial and Biocompatibility

Abstract

In this study, it was aimed to synthesize hydrogel based antibacterial, biocompatible and non-toxic wound dressing materials by solvent removal method usingpoly(vinylalcohol) (PVA), poly(vinylpyrolidone) (PVP) and nano pomegranate seed (PN).The morphology, swelling capacity, contact angle, antibacterial activity, biocompatibility and cytotoxicity of the synthesized films were determined. From the experimental findings, it was found that the PN particles were nano-sized, showed homogeneous and spherical distribution and improved the hydrophobic properties of the materials obtained by the addition of PN. And also, their swelling capacities were decreased with increased PN amount and all of the materials showed similar antibacterial activity, hemocompatibility and cytotoxicity.

Open access
Synthesis, growth and characterization of semiorganic nonlinear optical single crystal bis(thiourea) barium nitrate (BTBN) for frequency conversion

Abstract

A novel semiorganic nonlinear optical (NLO) crystal, bis(thiourea) barium nitrate (BTBN) was synthesized and grown by slow evaporation method. Structure of the new crystalline compound was confirmed by single crystal X-ray diffraction analysis and it showed that BTBN belongs to orthorhombic crystal system. The crystalline nature of the BTBN was confirmed by powder X-ray diffraction study. Important functional groups of BTBN were identified by FT-IR spectroscopic analysis. UV-Vis-NIR spectral study showed that the grown crystal is transparent in the entire visible region with low cut off wavelength of 304 nm. BTBN exhibits a SHG efficiency which is nearly 2.38 times higher than that of KDP. The BTBN crystal has high mechanical strength and belongs to soft category, which was confirmed by micorhardness study. The thermal stability of BTBN was determined from TGA and DTA thermal study which revealed that the BTBN crystal has thermal stability up to 243.1 °C. The surface properties and presence of elements was analyzed by SEM and EDAX study, respectively.

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Synthesis of new mesostructured cellular foams (MCFs) with NaY zeolite and their application to sorption of thorium ions

Abstract

The paper presents the new way of preparation of MCF foams with NaY zeolite. Significant changes in the amount of micro and mesopores in relation to the amount of NaY zeolite and 1,3,5-trimethylbenzene (TMB) added during the synthesis was observed. It suggests the possibility of controlling the micro/mesopores ratio by applying the proposed method. Environmental aspects of using new MCF/NaY foams is related to the adsorption of thorium ions (Th+4). The term of “MCF/NaY materials” refers to the general name of the material without referring to the content and state of zeolite. The obtained materials were highly effective in relation to Th+4. The adsorption capacity was greater when the number of micropores was lower. The dependence of adsorption capacity of Th+4 ions on aluminum atoms content was also confirmed.

Open access
Synthesis of single-crystalline Pb(Zr0.52Ti0.48)O3 nanocrystals by hydrothermal method

Abstract

PbZr0.52Ti0.48O3 nanocrystals were synthesized by a hydrothermal method. The effect of NaOH concentration, reaction temperature and time on nucleation and growth of PbZr0.52Ti0.48O3 nanocrystals was investigated. As the 0.05 mol/L PbZr0.52Ti0.48O3 precursors were heated at 200 °C for 21 h with NaOH concentration of 0.5 mol/L, the tetragonal PbZr0.52Ti0.48O3 nanocrystals were formed, and the grain size was more than 20 nm. With increasing the NaOH concentration from 0.5 to 1.5 mol/L, the grain size of PbZr0.52Ti0.48O3 nanocrystals decreased. When the precursors were heated at different temperatures (140 °C to 200 °C) for 21 h with 1.0 mol/L NaOH, single-phase PbZr0.52Ti0.48O3 nanocrystals were obtained at 160 °C to 200 °C. With increasing the reaction temperature from 160 °C to 200 °C, the grains size of PbZr0.52Ti0.48O3 nanocrystals increased from 5 nm to 9 nm. When the precursors were heated at 160 °C in different reaction times from 6 h to 21 h, the evolution from amorphous to crystalline PbZr0.52Ti0.48O3 nanocrystals in correlation with the reaction time was observed. Single crystalline PbZr0.52Ti0.48O3 nanocrystals with narrow size distribution (from 5 nm to 9 nm) were synthesized by controlling the NaOH concentration, reaction temperature and time. The obtained results can find potential application in preparing PbZr0.52Ti0.48O3 thin films on flexible substrates.

Open access