SYNTHESIS AND CHARACTERIZATION OF SPHERE-LIKE ZnS NANOCRYSTALS BY THERMOLYSIS OF A NEW COMPLEX PRECURSOR

2010 ◽  
Vol 24 (19) ◽  
pp. 2091-2099 ◽  
Author(s):  
JIANJUN ZHANG ◽  
JUNHONG DUAN

In this paper, the preparation and optical properties of sphere-like ZnS nanocrystals are reported. Pure and uniform cubic-phase sphere-like ZnS nanocrystals with grain sizes of 30–40 nm were synthesized by thermolysis of a new precursor complex ( enH 2)0.5[ Zn ( en )3]( SCN )3 (en = ethylenediamine) in nitrogen stream at 800°C. The as-synthesized products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS), respectively. The XRD analysis reveals the phase of ZnS with cubic zinc blende. UV-Vis and photoluminescence spectra (PL) were utilized to investigate the optical properties of sphere-like ZnS nanocrystals. By testing on UV-Vis spectra, it is concluded that the limiting wavelength of the ZnS nanocrystals is 320 nm and the band gap is 3.88 eV. In room temperature PL spectra, one strong emission peak centered at 322 nm is discovered, which could be attributed to the band to band transitions. The above-mentioned results showed that the thermolysis method is preferable for synthesizing high-quality sphere-like ZnS nanocrystals. The synthesized precursor could be used as morphological templates to prepare nanostructure inorganic compounds.

1997 ◽  
Vol 495 ◽  
Author(s):  
E. O. Bensadon ◽  
P. A. P. Nascente ◽  
L.O.S. Bulhões ◽  
E. C. Pereira

ABSTRACTA new methodology was developed to stabilized zirconia films at room temperature. The zirconium oxide films were prepared electrochemically by anodic oxidation of metallic zirconium at constant curcent density. X-ray diffraction (XRD) revealed the partial stabilization of the cubic phase in the ZrO2 films obtained in the presence of calcium. On the other hand, the films obtained in H3PO4 presented monoclinic phase. Scanning electron microscopy (SEM) showed that the oxide films obtained in calcium medium were porous, while the films obtained in H3PO4 were compact. X-ray photoelectron spectroscopy (XPS) identified ZrO2 and the intercalation of Na, N, P and CaO, as well as adventitious carbon. Using depth profiling, we observed that the concentrations of ZrO2, P and CaO increased with sputtering time.


Coatings ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 937
Author(s):  
Yingying Hu ◽  
Md Rasadujjaman ◽  
Yanrong Wang ◽  
Jing Zhang ◽  
Jiang Yan ◽  
...  

By reactive DC magnetron sputtering from a pure Ta target onto silicon substrates, Ta(N) films were prepared with different N2 flow rates of 0, 12, 17, 25, 38, and 58 sccm. The effects of N2 flow rate on the electrical properties, crystal structure, elemental composition, and optical properties of Ta(N) were studied. These properties were characterized by the four-probe method, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and spectroscopic ellipsometry (SE). Results show that the deposition rate decreases with an increase of N2 flows. Furthermore, as resistivity increases, the crystal size decreases, the crystal structure transitions from β-Ta to TaN(111), and finally becomes the N-rich phase Ta3N5(130, 040). Studying the optical properties, it is found that there are differences in the refractive index (n) and extinction coefficient (k) of Ta(N) with different thicknesses and different N2 flow rates, depending on the crystal size and crystal phase structure.


Nanomaterials ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 1969
Author(s):  
Riccardo Scarfiello ◽  
Elisabetta Mazzotta ◽  
Davide Altamura ◽  
Concetta Nobile ◽  
Rosanna Mastria ◽  
...  

The surface and structural characterization techniques of three atom-thick bi-dimensional 2D-WS2 colloidal nanocrystals cross the limit of bulk investigation, offering the possibility of simultaneous phase identification, structural-to-morphological evaluation, and surface chemical description. In the present study, we report a rational understanding based on X-ray photoelectron spectroscopy (XPS) and structural inspection of two kinds of dimensionally controllable 2D-WS2 colloidal nanoflakes (NFLs) generated with a surfactant assisted non-hydrolytic route. The qualitative and quantitative determination of 1T’ and 2H phases based on W 4f XPS signal components, together with the presence of two kinds of sulfur ions, S22− and S2−, based on S 2p signal and related to the formation of WS2 and WOxSy in a mixed oxygen-sulfur environment, are carefully reported and discussed for both nanocrystals breeds. The XPS results are used as an input for detailed X-ray Diffraction (XRD) analysis allowing for a clear discrimination of NFLs crystal habit, and an estimation of the exact number of atomic monolayers composing the 2D-WS2 nanocrystalline samples.


2020 ◽  
Vol 849 ◽  
pp. 113-118
Author(s):  
Yayat Iman Supriyatna ◽  
Slamet Sumardi ◽  
Widi Astuti ◽  
Athessia N. Nainggolan ◽  
Ajeng W. Ismail ◽  
...  

The purpose of this study is to characterize Lampung iron sand and to conduct preliminary experiments on the TiO2 synthesis which can be used for the manufacturing of functional food packaging. The iron sand from South Lampung Regency, Lampung Province that will be utilized as raw material. The experiment was initiated by sieving the iron sand on 80, 100, 150, 200 and 325 mesh sieves. Analysis using X-Ray Fluorescence (XRF) to determine the element content and X-Ray Diffraction (XRD) to observe the mineralization of the iron sand was conducted. The experiment was carried out through the stages of leaching, precipitation, and calcination. Roasting was applied firstly by putting the iron sand into the muffle furnace for 5 hours at a temperature of 700°C. Followed by leaching using HCl for 48 hours and heated at 105°C with a stirring speed of 300 rpm. The leaching solution was filtered with filtrate and solid residue as products. The solid residue was then leached using 10% H2O2 solution. The leached filtrate was heated at 105°C for 40 minutes resulting TiO2 precipitates (powder). Further, the powder was calcined and characterized. Characterization of raw material using XRF shows the major elements of Fe, Ti, Mg, Si, Al and Ca. The highest Ti content is found in mesh 200 with 9.6%, while iron content is about 80.7%. While from the XRD analysis, it shows five mineral types namely magnetite (Fe3O4), Rhodonite (Mn, Fe, Mg, Ca) SiO3, Quart (SiO2), Ilmenite (FeOTiO2) and Rutile (TiO2). The preliminary experiment showed that the Ti content in the synthesized TiO2 powder is 21.2%. The purity of TiO2 is low due to the presence of Fe metal which is dissolved during leaching, so that prior to precipitation purification is needed to remove impurities such as iron and other metals.


2015 ◽  
Vol 2015 ◽  
pp. 1-6 ◽  
Author(s):  
YiChao Yan ◽  
Wei Shi ◽  
HongChuan Jiang ◽  
Jie Xiong ◽  
WanLi Zhang ◽  
...  

The redox reaction between Al and metallic oxide has its advantage compared with intermetallic reaction and Al/NiO nanomutlilayers are a promising candidate for enhancing the performance of energetic igniter. Al/NiO nanomutlilayers with different modulation periods are prepared on alumina substrate by direct current (DC) magnetron sputtering. The thicknesses of each period are 250 nm, 500 nm, 750 nm, 1000 nm, and 1500 nm, respectively, and the total thickness is 3 μm. The X-ray diffraction (XRD) and scanning electron microscope (SEM) results of the as-deposited Al/NiO nanomutlilayers show that the NiO films are amorphous and the layered structures are clearly distinguished. The X-ray photoelectron spectroscopy (XPS) demonstrates that the thickness of Al2O3increases on the side of Al monolayer after annealing at 450°C. The thermal diffusion time becomes greater significantly as the amount of thermal boundary conductance across the interfaces increases with relatively smaller modulation period. Differential scanning calorimeter (DSC) curve suggests that the energy release per unit mass is below the theoretical heat of the reaction due to the nonstoichiometric ratio between Al and NiO and the presence of impurities.


2013 ◽  
Vol 873 ◽  
pp. 152-157
Author(s):  
Long Long Chen ◽  
Jun Ming Li ◽  
Xiao Min Gong ◽  
Jian Li

Using a chemically induced transition in an FeCl2 solution, γ-Fe2O3 nanoparticles can be prepared from an amorphous precursor composed of FeOOH and Mg (OH)2. Surface modification by adding ZnCl2 during liquid-phase synthesis was attempted. The magnetization, morphology, crystal structure, and chemical species of as-prepared samples were characterized by vibrating sample magnetometer (VSM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray energy-dispersive spectroscopy (EDX), and X-ray photoelectron spectroscopy (XPS). The experimental results showed that the surface of the γ-Fe2O3 nanoparticles can be modified by adding ZnCl2 to form composite nanoparticles with a γ-Fe2O3/ZnFe2O4 ferrite core coated with Zn (OH)2 and absorbed FeCl36H2O; this modification can be enhanced by additional NaOH.


2020 ◽  
Author(s):  
Sahar. Mokhtari ◽  
Anthony.W. Wren

AbstractThis study addresses issues with currently used bone adhesives, by producing novel glass based skeletal adhesives through modification of the base glass composition to include copper (Cu) and by characterizing each glass with respect to structural changes. Bioactive glasses have found applications in fields such as orthopedics and dentistry, where they have been utilized for the restoration of bone and teeth. The present work outlines the formation of flexible organic-inorganic polyacrylic acid (PAA) – glass hybrids, commercial forms are known as glass ionomer cements (GICs). Initial stages of this research will involve characterization of the Cu-glasses, significant to evaluate the properties of the resulting adhesives. Scanning electron microscopy (SEM) of annealed Cu glasses indicates the presence of partial crystallization in the glass. The structural analysis of the glass using Raman suggests the formation of CuO nanocrystals on the surface. X-ray diffraction (XRD) pattern and X-ray photoelectron spectroscopy (XPS) further confirmed the formation of crystalline CuO phases on the surface of the annealed Cu-glass. The setting reaction was studied using Fourier transform infrared spectroscopy (ATR-FTIR). The mechanical properties of the Cu containing adhesives exhibited gel viscoelastic behavior and enhanced mechanical properties when compared to the control composition. Compression data indicated the Cu glass adhesives were efficient at energy dissipation due to the reversible interactions between CuO nano particles and PAA polymer chains.


Chemija ◽  
2019 ◽  
Vol 30 (2) ◽  
Author(s):  
Andrius Laurikėnas ◽  
Fatma Yalçin ◽  
Robertas Žilinskas ◽  
Ayse Uztetik Morkan ◽  
Albinas Žilinskas ◽  
...  

The solvothermal synthesis between Me(NO3)x ∙ yH2O (Mex+ = Fe3+, Ni2+, Mn2+, Co2+, Cu2+) and respectively 4-nitrosalycilic (4NSA) and 5-sulfosalicylic (5SSA) acids produced hybrid organic-inorganic compounds composed of Mex+ ions and organic fragments which include three different functional groups, carboxylic, hydroxyl and sulfonic, each coordinated to the Mex+ ions. The phase and chemical composition, microstructure and properties of Me2(H2O)4(5SSA)3·DMF and Me2(H2O)4(4NSA)2·DMF (DMF – dimethylformamide) hybrid compounds were evaluated and discussed. The synthesised materials were characterised by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) and nuclear magnetic resonance (NMR) spectroscopy. The catalytic properties of the obtained compounds were also investigated.


2000 ◽  
Vol 15 (10) ◽  
pp. 2076-2079
Author(s):  
Chika Nozaki ◽  
Takashi Yamada ◽  
Kenji Tabata ◽  
Eiji Suzuki

Synthesis of a rutile-type lead-substituted tin oxide with (110) face was investigated. The characterization was performed by x-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive x-ray spectroscopy, infrared spectroscopy, x-ray photoelectron spectroscopy, and Brunauer–Emmett–Teller surface area measurements. The homogeneous rutile-type lead-substituted tin oxide was obtained until 4.1 mol% of tin was substituted with lead. The surface of obtained oxide had a homogeneously lead-substituted (110) face.


Author(s):  
M.T. Blatchford ◽  
A.J. Horlock ◽  
D.G. McCartney ◽  
P.H. Shipway ◽  
J.V. Wood

Abstract In this paper, the production of NiCr-TiC powder by SHS, suitable for HVOF spraying, is discussed together with results on the microstructure and coating properties. Compacts for SHS were prepared by mixing elemental Ti and C with pre-alloyed Ni-20wt.% Cr powder to give an overall composition of 35wt.% NiCr and 65wt.% TiC. These were then ignited and a self-sustaining reaction proceeded to completion. Reacted compacts were crushed, sieved, and classified to give feedstock powders in size ranges of 10-45 µm and 45-75 µm. All powder was characterized prior to spraying based on particle size distribution, x-ray diffraction (XRD), and scanning electron microscopy (SEM/EDS). Thermal spraying was performed using both H2 and C3H6 as fuel gases in a UTP/Miller Thermal HVOF system. The resulting coatings were characterized by SEM and XRD analysis, and the microstructures correlated with powder size and spray conditions. Abrasive wear was determined by a modified 'dry sand rubber wheel' (DSRW) test and wear rates were measured. It has been found that wear rates comparable to those of HVOF sprayed WC-17wt% Co coatings can be achieved.


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