Abstract: The present paper discusses the selection of process
parameters for obtaining optimal nanocrystallites size in the CuOZrO2
catalyst. There are some parameters changing the inorganic
structure which have an influence on the role of hydrolysis and
condensation reaction. A statistical design test method is
implemented in order to optimize the experimental conditions of
CuO-ZrO2 nanoparticles preparation. This method is applied for the
experiments and L16 orthogonal array standard. The crystallites size
is considered as an index. This index will be used for the analysis in
the condition where the parameters vary. The effect of pH, H2O/
precursor molar ratio (R), time and temperature of calcination,
chelating agent and alcohol volume are particularity investigated
among all other parameters. In accordance with the results of
Taguchi, it is found that temperature has the greatest impact on the
particle size. The pH and H2O/ precursor molar ratio have low
influences as compared with temperature. The alcohol volume as
well as the time has almost no effect as compared with all other
parameters. Temperature also has an influence on the morphology
and amorphous structure of zirconia. The optimal conditions are
determined by using Taguchi method. The nanocatalyst is studied by
DTA-TG, XRD, EDS, SEM and TEM. The results of this research
indicate that it is possible to vary the structure, morphology and
properties of the sol-gel by controlling the above-mentioned
parameters.
Abstract: Solid dispersions (SD) of curcuminpolyvinylpyrrolidone
in the ratio of 1:2, 1:4, 1:5, 1:6, and 1:8 were
prepared in an attempt to increase the solubility and dissolution.
Solubility, dissolution, powder X-ray diffraction (XRD), differential
scanning calorimetry (DSC) and Fourier transform infrared
spectroscopy (FTIR) of solid dispersions, physical mixtures (PM)
and curcumin were evaluated. Both solubility and dissolution of
curcumin solid dispersions were significantly greater than those
observed for physical mixtures and intact curcumin. The powder
X-ray diffractograms indicated that the amorphous curcumin was
obtained from all solid dispersions. It was found that the optimum
weight ratio for curcumin:PVP K-30 is 1:6. The 1:6 solid dispersion
still in the amorphous from after storage at ambient temperature for 2
years and the dissolution profile did not significantly different from
freshly prepared.
Abstract: The crystallization kinetics and phase transformation
of SiO2.Al2O3.0,56P2O5.1,8CaO.0,56CaF2 glass have been
investigated using differential thermal analysis (DTA), x-ray
diffraction (XRD), and scanning electron microscopy (SEM). Glass
samples were obtained by melting the glass mixture at 14500С/120
min. in platinum crucibles. The mixture were prepared from
chemically pure reagents: SiO2, Al(OH)3, H3PO4, CaCO3 and CaF2.
The non-isothermal kinetics of crystallization was studied by
applying the DTA measurements carried out at various heating rates.
The activation energies of crystallization and viscous flow were
measured as 348,4 kJ.mol–1 and 479,7 kJ.mol–1 respectively. Value of
Avrami parameter n ≈ 3 correspond to a three dimensional of crystal
growth mechanism. The major crystalline phase determined by XRD
analysis was fluorapatite (Ca(PO4)3F) and as the minor phases –
fluormargarite (CaAl2(Al2SiO2)10F2) and vitlokite (Ca9P6O24). The
resulting glass-ceramic has a homogeneous microstructure, composed
of prismatic crystals, evenly distributed in glass phase.
Abstract: Using steelmaking slag as a raw material, aragonite superstructure product had been synthesized via an indirect CO2 mineral sequestration rout. It mainly involved two separate steps, in which the element of calcium is first selectively leached from steelmaking slag by a novel leaching media consisting of organic solvent Tributyl phosphate (TBP), acetic acid, and ultra-purity water, followed by enhanced carbonation in a separate step for aragonite superstructure production as well as efficiency recovery of leaching media. Based on the different leaching medium employed in the steelmaking slag leaching process, two typical products were collected from the enhanced carbonation step. The products were characterized by X-ray powder diffraction (XRD) and scanning electron microscopy (SEM), respectively. It reveals that the needle-like aragonite crystals self-organized into aragonite superstructure particles including aragonite microspheres as well as dumbbell-like spherical particles, can be obtained from the steelmaking slag with the purity over 99%.
Abstract: The systematic manipulations of shapes and sizes of
inorganic compounds greatly benefit the various application fields
including optics, magnetic, electronics, catalysis and medicine.
However shape control has been much more difficult to achieve.
Hence exploration of novel method for the preparation of differently
shaped nanoparticles is challenging research area. II-VI group of
semiconductor cadmium sulphide (CdS) nanostructure with different
morphologies (such as, acicular like, mesoporous, spherical shapes)
and of crystallite sizes vary from 11 to 16 nm were successfully
synthesized by chemical aqueous precipitation of Cd2+ ions with
homogeneously released S2- ions from decomposition of cadmium
sulphate (CdSO4) and thioacetamide (CH3CSNH2) by annealing at
different radiations (microwave, ultrasonic and sunlight) with matter
and systematic research has been done for various factors affecting
the controlled growth rate of CdS nanoparticles. The obtained
nanomaterials have been characterized by X-ray Diffraction (XRD),
Fourier Transform Infrared Spectroscopy (FTIR),
Thermogravometric (DSC-TGA) analysis and Scanning Electron
Microscopy (SEM). The result indicates that on increasing the
reaction time particle size increases but on increasing the molar ratios
grain size decreases.
Abstract: In this paper the combination of thermal oxidation and
electrochemical anodizing processes is used to produce titanium
oxide layers. The response of titanium alloy Ti6Al4V to oxidation
processes at various temperatures and electrochemical anodizing in
various voltages are investigated. Scanning electron microscopy
(SEM); X-Ray Diffraction (XRD) and porosity determination have
been used to characterize the oxide layer thickness, surface
morphology, oxide layer-substrate adhesion and porosity. In the first
experiment, samples modified by thermal oxidation process then
followed by electrochemical anodizing. Second experiment consists
of surfaces modified by electrochemical anodizing process and then
followed by thermal oxidation. The first method shows better
properties than other one. In second experiment, Surfaces modified
were achieved by thicker and more adherent thick oxide layers on
titanium surface. The existence of an electrochemical anodized oxide
layer did not improve the adhesion of thermal oxide layer. The high
temperature, thermal formation of an oxide layer leads to a coarse
oxide grain morphology and a complete oxidative particle. In
addition, in high temperature oxidation porosity content is increased.
The oxide layer of thermal oxidation and electrochemical anodizing
processes; on Ti–6Al–4V substrate was covered with different
colored oxide layers.
Abstract: Un-doped GaN film of thickness 1.90 mm, grown on
sapphire substrate were uniformly implanted with 325 keV Mn+ ions
for various fluences varying from 1.75 x 1015 - 2.0 x 1016 ions cm-2 at
3500 C substrate temperature. The structural, morphological and
magnetic properties of Mn ion implanted gallium nitride samples
were studied using XRD, AFM and SQUID techniques. XRD of the
sample implanted with various ion fluences showed the presence of
different magnetic phases of Ga3Mn, Ga0.6Mn0.4 and Mn4N.
However, the compositions of these phases were found to be
depended on the ion fluence. AFM images of non-implanted sample
showed micrograph with rms surface roughness 2.17 nm. Whereas
samples implanted with the various fluences showed the presence of
nano clusters on the surface of GaN. The shape, size and density of
the clusters were found to vary with respect to ion fluence. Magnetic
moment versus applied field curves of the samples implanted with
various fluences exhibit the hysteresis loops. The Curie temperature
estimated from zero field cooled and field cooled curves for the
samples implanted with the fluence of 1.75 x 1015, 1.5 x 1016 and 2.0
x 1016 ions cm-2 was found to be 309 K, 342 K and 350 K
respectively.
Abstract: ZnS nanoparticles of different size have been
synthesized using a colloidal particles method. Zns nanoparticles
prepared with capping agent (mercaptoethanol) then were
characterized using X-ray diffraction (XRD) and UV-Vis
spectroscopy. The particle size of the nanoparticles calculated from
the XRD patterns has been found in the range 1.85-2.44nm.
Absorption spectra have been obtained using UV-Vis
spectrophotometer to find the optical band gap and the obtained
values have been founded to being range 3.83-4.59eV. It was also
found that energy band gap increase with the increase in molar
capping agent solution.
Abstract: The present paper reports results of an experimental
program conducted to study performance of fly ash based
geopolymer pastes at elevated temperature. Three series of
geopolymer pastes differing in Na2O content (8.5%, 10% and 11.5%)
were manufactured by activating low calcium fly ash with a mixture
of sodium hydroxide and sodium silicate solution. The paste
specimens were subjected to temperatures as high as 900oC and the
behaviour at elevated temperatures were investigated on the basis of
physical appearance, weight losses, residual strength, shrinkage
measurements and sorptivity tests at different temperatures. Scanning
electron microscopy along with EDX and XRD tests were also
conducted to examine microstructure and mineralogical changes
during the thermal exposure. Specimens which were initially grey
turned reddish accompanied by appearance of small cracks as the
temperature increased to 900oC. Loss of weight was more in
specimens manufactured with highest Na2O content. Geopolymer
paste specimen containing minimum Na2O performed better than
those with higher Na2O content in terms of residual compressive
strength.
Abstract: n-CdO/p-Si heterojunction diode was fabricated using
sol-gel spin coating technique which is a low cost and easily scalable
method for preparing of semiconductor films. The structural and
morphological properties of CdO film were investigated. The X-ray
diffraction (XRD) spectra indicated that the film was of
polycrystalline nature. The scanning electron microscopy (SEM)
images indicate that the surface morphology CdO film consists of the
clusters formed with the coming together of the nanoparticles. The
electrical characterization of Au/n-CdO/p–Si/Al heterojunction diode
was investigated by current-voltage. The ideality factor of the diode
was found to be 3.02 for room temperature. The reverse current of
the diode strongly increased with illumination intensity of 100
mWcm-2 and the diode gave a maximum open circuit voltage Voc of
0.04 V and short-circuits current Isc of 9.92×10-9 A.
Abstract: In this investigation, anatase TiO2 thin films were
grown by radio frequency magnetron sputtering on glass substrates at
a high sputtering pressure and room temperature. The anatase films
were then annealed at 300-600 °C in air for a period of 1 hour. To
examine the structure and morphology of the films, X-ray diffraction
(XRD) and atomic force microscopy (AFM) methods were used
respectively. From X-ray diffraction patterns of the TiO2 films, it was
found that the as-deposited film showed some differences compared
with the annealed films and the intensities of the peaks of the
crystalline phase increased with the increase of annealing
temperature. From AFM images, the distinct variations in the
morphology of the thin films were also observed. The optical
constants were characterized using the transmission spectra of the
films obtained by UV-VIS-IR spectrophotometer. Besides, optical
thickness of the film deposited at room temperature was calculated
and cross-checked by taking a cross-sectional image through SEM.
The optical band gaps were evaluated through Tauc model. It was
observed that TiO2 films produced at room temperatures exhibited
high visible transmittance and transmittance decreased slightly with
the increase of annealing temperatures. The films were found to be
crystalline having anatase phase. The refractive index of the films
was found from 2.31-2.35 in the visible range. The extinction
coefficient was nearly zero in the visible range and was found to
increase with annealing temperature. The allowed indirect optical
band gap of the films was estimated to be in the range from 3.39 to
3.42 eV which showed a small variation. The allowed direct band
gap was found to increase from 3.67 to 3.72 eV. The porosity was
also found to decrease at a higher annealing temperature making the
film compact and dense.
Abstract: Highly ordered TiO2 nanotube (TNT) arrays were
fabricated onto a pre-treated titanium foil by anodic oxidation with a
voltage of 20V in phosphoric acid/sodium fluoride electrolyte. A pretreatment
of titanium foil involved washing with acetone,
isopropanol, ethanol and deionized water. Carbon doped TiO2
nanotubes (C-TNT) was fabricated 'in-situ' with the same method in
the presence of polyvinyl alcohol and urea as carbon sources. The
affects of polyvinyl alcohol concentration and oxidation time on the
composition, morphology and structure of the C-TN were studied by
FE-SEM, EDX and XRD techniques. FESEM images of the
nanotubes showed uniform arrays of C-TNTs. The density and
microstructures of the nanotubes were greatly affected by the content
of PVA. The introduction of the polyvinyl alcohol into the electrolyte
increases the amount of C content inside TiO2 nanotube arrays
uniformly. The influence of carbon content on the photo-current of
C-TNT was investigated and the I-V profiles of the nanotubes were
established. The preliminary results indicated that the 'in-situ'
doping technique produced a superior quality nanotubes compared to
post doping techniques.
Abstract: Commercial nanocomposite food packaging type nano-silver containers were characterised using scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The presence of nanoparticles consistent with the incorporation of 1% nano-silver (Ag) and 0.1% titanium dioxide (TiO2) nanoparticle into polymeric materials formed into food containers was confirmed. Both nanomaterials used in this type of packaging appear to be embedded in a layered configuration within the bulk polymer. The dimensions of the incorporated nanoparticles were investigated using X-ray diffraction (XRD) and determined by calculation using the Scherrer Formula; these were consistent with Ag and TiO2 nanoparticles in the size range 20-70nm both were spherical shape nanoparticles. Antimicrobial assessment of the nanocomposite container has also been performed and the results confirm the antimicrobial activity of Ag and TiO2 nanoparticles in food packaging containers. Migration assessments were performed in a wide range of food matrices to determine the migration of nanoparticles from the packages. The analysis was based upon the relevant European safety Directives and involved the application of inductively coupled plasma mass spectrometry (ICP-MS) to identify the range of migration risk. The data pertain to insignificance levels of migration of Ag and TiO2 nanoparticles into the selected food matrices.
Abstract: Adsorption of Toluidine blue dye from aqueous solutions onto Neem Leaf Powder (NLP) has been investigated. The surface characterization of this natural material was examined by Particle size analysis, Scanning Electron Microscopy (SEM), Fourier Transform Infrared (FTIR) spectroscopy and X-Ray Diffraction (XRD). The effects of process parameters such as initial concentration, pH, temperature and contact duration on the adsorption capacities have been evaluated, in which pH has been found to be most effective parameter among all. The data were analyzed using the Langmuir and Freundlich for explaining the equilibrium characteristics of adsorption. And kinetic models like pseudo first- order, second-order model and Elovich equation were utilized to describe the kinetic data. The experimental data were well fitted with Langmuir adsorption isotherm model and pseudo second order kinetic model. The thermodynamic parameters, such as Free energy of adsorption (AG"), enthalpy change (AH') and entropy change (AS°) were also determined and evaluated.
Abstract: In this study, hydroxyapatite (HA) composites are
prepared on addition of 30%CaO-30%P2O5-40%Na2 O based glass to
pure HA, in proportion of 2, 5, and 10 wt %. Each composition was
sintered over a range of temperatures. The quantitative phase
analysis was carried out using XRD and the microstructures were
studied using SEM. The density, microhardness, and compressive
strength have shown increase with the increasing amount of glass
addition. The resulting composites have chemical compositions that
are similar to the inorganic constituent of the mineral part of bone,
and constitutes trace elements like Na. X-ray diffraction showed no
decomposition of HA to secondary phases, however, the glass
reinforced-HA composites contained a HA phase and variable
amounts of tricalcium phosphate phase, depending on the amount of
bioglass added. The HA-composite material exhibited higher
compressive strength compared to sintered HA. The HA composite
reinforced with 10 wt % bioglass showed highest bioactivity level.
Abstract: Palm shell obtained from coastal part of southern
India was studied for the removal for the adsorption of Hg (II) ions.
Batch adsorption experiments were carried out as a function of pH,
concentration of Hg (II) ions, time, temperature and adsorbent dose.
Maximum removal was seen in the range pH 4.0- pH 7.0. The palm
shell powder used as adsorbent was characterized for its surface area,
SEM, PXRD, FTIR, ion exchange capacity, moisture content, and
bulk density, soluble content in water and acid and pH. The
experimental results were analyzed using Langmuir I, II, III, IV and
Freundlich adsorption isotherms. The batch sorption kinetics was
studied for the first order reversible reaction, pseudo first order;
pseudo second order reaction and the intra-particle diffusion reaction.
The biomass was successfully used for removal Hg (II) from
synthetic and industrial effluents and the technique appears
industrially applicable and viable.
Abstract: Three alumina-supported Pt-Sn catalysts have been
prepared by means of co-impregnation and characterized by XRD and
N2 adsorption. The influence of catalyst composition and reaction
conditions on the conversion and selectivity were investigated in the
hydrogenation of acetic acid in an isothermal integral fixed bed
reactor. The experiments were performed on the temperature interval
468-548 K, liquid hourly space velocity (LHSV) of 0.3-0.7h-1,
pressures between 1.0 and 5.0Mpa. A good compromise of
0.75%Pt-1.5%Sn can act as an optimized acetic acid hydrogenation
catalyst, and the conversion and selectivity can be tuned through the
variation of reaction conditions.
Abstract: This paper presents a experiment to estimate the
influences of cutting conditions in microstructure changes of
machining austenitic 304 stainless steel, especially for wear insert. The
wear insert were prefabricated with a width of 0.5 mm. And the forces,
temperature distribution, RS, and microstructure changes were
measured by force dynamometer, infrared thermal camera, X-ray
diffraction, XRD, SEM, respectively. The results told that the different
combinations of machining condition have a significant influence on
machined surface microstructure changes. In addition to that, the
ANOVA and AOMwere used to tell the different influences of cutting
speed, feed rate, and wear insert.
Abstract: Copper sulfide nanoparticles (CuS) were successfully synthesized by the pulsed plasma in liquid method, using two copper rod electrodes submerged in molten sulfur. Low electrical energy and no high temperature were applied for synthesis. Obtained CuS nanoparticles were then analyzed by means of X-ray diffraction, Low and High Resolution Transmission Electron Microscopy, Electron Diffraction, X-ray Photoelectron, Raman Spectroscopies and Field Emission Scanning Electron Microscopy. XRD analysis revealed peaks for CuS with hexagonal phase composition. TEM and HRTEM studies showed that sizes of CuS nanoparticles ranged between 10-60 nm, with the average size of about 20 nm. Copper sulfide nanoparticles have short nanorod-like structure. Raman spectroscopy found peak for CuS at 474.2cm-1of Raman region.
Abstract: Magnesium wastes and scraps, one of the metal wastes, are produced by many industrial activities, all over the world. Their growing size is becoming a future problem for the world. In this study, the use of magnesium wastes as a raw material in the production of the magnesium borate hydrates are aimed. The method used in the experiments is hydrothermal synthesis. The conditions are set to, waste magnesium to B2O3, 1:3 as a molar ratio. Four different reaction times are studied which are 30, 60, 120 and 240 minutes. For the identification analyses X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Raman spectroscopy techniques are used. As a result at all the reaction times magnesium borate hydrates are synthesized and the most crystalline forms are obtained at a reaction time of 120 minutes. The overall yields of the production are found between the values of 65-80 %.