Abstract: In this work, obtaining methods of ultrafine alumina
powdery composites and high temperature pressing technology of
matrix ceramic composites with different compositions have been
discussed. Alumina was obtained by solution combustion synthesis
and sol-gel methods. Metal carbides containing powdery composites
were obtained by homogenization of finishing powders in nanomills,
as well as by their single-step high temperature synthesis .Different
types of matrix ceramics composites (α-Al2O3-ZrO2-Y2O3, α-Al2O3-
Y2O3-MgO, α-Al2O3-SiC-Y2O3, α-Al2O3-WC-Co-Y2O3, α-Al2O3-
B4C-Y2O3, α-Al2O3- B4C-TiB2 etc.) were obtained by using OXYGON
furnace. Consolidation of powders were carried out at 1550-
1750°C (hold time - 1 h, pressure - 50 MPa). Corundum ceramics
samples have been obtained and characterized by high hardness and
fracture toughness, absence of open porosity, high corrosion
resistance. Their density reaches 99.5-99.6% TD. During the work,
the following devices have been used: High temperature vacuum
furnace OXY-GON Industries Inc (USA), Electronic Scanning
Microscopes Nikon Eclipse LV 150, Optical Microscope NMM-
800TRF, Planetary mill Pulverisette 7 premium line, Shimadzu
Dynamic Ultra Micro Hardness Tester DUH-211S, Analysette 12
Dynasizer.
Abstract: Nanoporous g-Al2O3 samples were synthesized via a sol-gel technique, introducing changes in the Yoldas´ method. The aim of the work was to achieve an effective control of the nanostructure properties and morphology of the final g-Al2O3. The influence of the reagent temperature during the hydrolysis was evaluated in case of water at 5 ºC and 98 ºC, and alkoxide at -18 ºC and room temperature. Sol-gel transitions were performed at 120 ºC and room temperature. All g-Al2O3 samples were characterized by X-ray diffraction, nitrogen adsorption and thermal analysis. Our results showed that temperature of both water and alkoxide has not much influence on the nanostructure of the final g-Al2O3, thus giving a structure very similar to that of samples obtained by the reference method as long as the reaction temperature above 75 ºC is reached soon enough. XRD characterization showed diffraction patterns corresponding to g-Al2O3 for all samples. Also BET specific area values (253-280 m2/g) were similar to those obtained by Yoldas’s original method. The temperature of the sol-gel transition does not affect the resulting sample structure, and crystalline boehmite particles were identified in all dried gels. We analyzed the reproducibility of the samples’ structure by preparing different samples under identical conditions; we found that performing the sol-gel transition at 120 ºC favors the production of more reproducible samples and also reduces significantly the time of the sol-gel reaction.
Abstract: Lithium niobate (LiNbO3) nanostructures are prepared on quartz substrate by the sol-gel method. They have been deposited with different molarity concentration and annealed at 500°C. These samples are characterized and analyzed by X-ray diffraction (XRD), Scanning Electron Microscope (SEM) and Atomic Force Microscopy (AFM). The measured results showed an importance increasing in molarity concentrations that indicate the structure starts to become crystal, regular, homogeneous, well crystal distributed, which made it more suitable for optical waveguide application.
Abstract: Nanocrystalline TiO2 particles were successfully synthesized via sol-gel and sonochemical combination using titanium tetraisopropoxide as a precursor at lower temperature for a short time. The effect of the reaction parameters (hydrolysis media, acid media, and reaction temperatures) on the synthesis of TiO2 particles were investigated in the present study. Characterizations of synthesized samples were prepared by X-ray diffraction (XRD) analysis. It was shown that the reaction parameters played a significant role in the synthesis of TiO2 particles.
Abstract: In this study, the effects and interactions of reaction
time and capping agent assistance during sol-gel synthesis of
magnesium substituted hydroxyapatite nanopowder (MgHA) on
hydroxyapatite (HA) to β-tricalcium phosphate (β-TCP) ratio, Ca/P
ratio and mean crystallite size was examined experimentally as well
as through statistical analysis. MgHA nanopowders were synthesized
by sol-gel technique at room temperature using aqueous solution of
calcium nitrate tetrahydrate, magnesium nitrate hexahydrate and
potassium dihydrogen phosphate as starting materials. The reaction
time for sol-gel synthesis was varied between 15 to 60 minutes. Two
process routes were followed with and without addition of
triethanolamine (TEA) in the solutions. The elemental compositions
of as-synthesized powders were determined using X-ray fluorescence
(XRF) spectroscopy. The functional groups present in the assynthesized
MgHA nanopowders were established through Fourier
Transform Infrared Spectroscopy (FTIR). The amounts of phases
present, Ca/P ratio and mean crystallite sizes of MgHA nanopowders
were determined using X-ray diffraction (XRD). The HA content in
biphasic mixture of HA and β-TCP and Ca/P ratio in as-synthesized
MgHA nanopowders increased effectively with reaction time of sols
(p0.15, two way ANOVA). The MgHA nanopowders
synthesized with TEA assistance exhibited 14 nm lower crystallite
size (p
Abstract: In this research, thorium dioxide mesoporous
nanocrystalline powder was synthesized through the sol-gel method
using hydrated thorium nitrate and ammonium hydroxide as starting
materials and Triton X100 as surfactant. ThO2 gel was characterized
by thermogravimetric (TGA), and prepared ThO2 powder was
subjected to scanning electron microscopy (SEM), X-ray diffraction
(XRD), and Brunauer-Emett-Teller (BET) analyses studies. Detailed
analyses show that prepared powder consisted of phase with the
space group Fm3m of thoria and its crystalline size was 12.6 nm. The
thoria possesses 16.7 m2/g surface area and the pore volume and size
calculated to be 0.0423 cc/g and 1.947 nm, respectively.
Abstract: Nanofibers of PVA /nickel nitrate/silica/alumina
izopropoxide/boric acid composite were prepared by using sol-gel
processing and electrospinning technique. By high temperature
calcinations of the above precursor fibers, nanofibers of
NiO/Al2O3/B2O3/SiO2 composite with diameters about 500 nm
could be successfully obtained. The fibers were characterized by
XRD and SEM analyses.
Abstract: It is well known that in recent years magnetic
materials have received increased attention due to their properties.
For this reason a significant number of patents that were published
during the last decade are oriented towards synthesis and study of
such materials. The aim of this work is to create and study ferrite
nanocrystalline materials with spinel structure, using sol-gel
technology with participation of auto-combustion. This method is
perspective in that it is a cheap and low-temperature technique that
allows for the fine control on the product’s chemical composition.
Abstract: Composite material based on Fe3Si micro-particles
and Mn-Zn nano-ferrite was prepared using powder metallurgy
technology. The sol-gel followed by autocombustion process was
used for synthesis of Mn0.8Zn0.2Fe2O4 ferrite. 3 wt.% of mechanically
milled ferrite was mixed with Fe3Si powder alloy. Mixed micro-nano
powder system was homogenized by the Resonant Acoustic Mixing
using ResodynLabRAM Mixer. This non-invasive homogenization
technique was used to preserve spherical morphology of Fe3Si
powder particles. Uniaxial cold pressing in the closed die at pressure
600 MPa was applied to obtain a compact sample. Microwave
sintering of green compact was realized at 800°C, 20 minutes, in air.
Density of the powders and composite was measured by
Hepycnometry. Impulse excitation method was used to measure
elastic properties of sintered composite. Mechanical properties were
evaluated by measurement of transverse rupture strength (TRS) and
Vickers hardness (HV). Resistivity was measured by 4 point probe
method. Ferrite phase distribution in volume of the composite was
documented by metallographic analysis.
It has been found that nano-ferrite particle distributed among
micro- particles of Fe3Si powder alloy led to high relative density
(~93%) and suitable mechanical properties (TRS >100 MPa, HV
~1GPa, E-modulus ~140 GPa) of the composite. High electric
resistivity (R~6.7 ohm.cm) of prepared composite indicate their
potential application as soft magnetic material at medium and high
frequencies.
Abstract: Thin ZnO films are deposited on glass substrates via
sol–gel method and dip-coating. The films are prepared from zinc
acetate dehydrate as a starting reagent. After that the as-prepared
ZnO sol is aged for different periods (0, 1, 3, 5, 10, 15 and 30 days).
Nanocrystalline thin films are deposited from various sols. The
effect ZnO sols aging time on the structural and photocatalytic
properties of the films is studied. The films surface is studied by
Scanning Electron Microscopy. The effect of the aging time of the
starting solution is studied in the photocatalytic degradation of
Reactive Black 5 (RB5) by UV-vis spectroscopy. The experiments
are conducted upon UV-light illumination and in complete darkness.
The variation of the absorption spectra shows the degradation of RB5
dissolved in water, as a result of the reaction, occurring on the surface
of the films and promoted by UV irradiation. The initial
concentrations of dye (5, 10 and 20 ppm) and the effect of the aging
time are varied during the experiments. The results show, that the
increasing aging time of starting solution with respect to ZnO
generally promotes photocatalytic activity. The thin films obtained
from ZnO sol, which is aged 30 days have best photocatalytic
degradation of the dye (97,22%) in comparison with the freshly
prepared ones (65,92%). The samples and photocatalytic
experimental results are reproducible. Nevertheless, all films exhibit
a substantial activity in both UV light and darkness, which is
promising for the development of new ZnO photocatalysts by sol-gel
method.
Abstract: The contact resistance between source/drain electrodes
and semiconductor layer is an important parameter affecting electron
transporting performance in the thin film transistor (TFT). In this
work, we introduced a transparent and the solution prossable
single-walled carbon nanotube (SWCNT)/Al-doped ZnO nano particle
(AZO NP) bilayer electrodes showing low contact resistance with
indium-oxide (In2O3) sol gel thin film. By inserting low work function
AZO NPs into the interface between the SWCNTs and the In2O3 which
has a high energy barrier, we could obtain an electrical Ohmic contact
between them. Finally, with the SWCNT-AZO NP bilayer electrodes,
we successfully fabricated a TFT showing a field effect mobility of
5.38 cm2/V·s at 250°C.
Abstract: TiO2 thin films have been prepared by the sol-gel dipcoating
technique in order to elaborate antireflective thin films for
monocrystalline silicon (mono-Si). The titanium isopropoxyde was
chosen as a precursor with hydrochloric acid as a catalyser for
preparing a stable solution. The optical properties have been tailored
with varying the solution concentration, the withdrawn speed, and the
heat-treatment. We showed that using a TiO2 single layer with 64.5
nm in thickness, heat-treated at 450°C or 300°C reduces the mono-Si
reflection at a level lower than 3% over the broadband spectral
domains [669-834] nm and [786-1006] nm respectively. Those latter
performances are similar to the ones obtained with double layers of
low and high refractive index glasses respectively.
Abstract: In this research, waterglass based aerogel powder was
prepared by sol–gel process and ambient pressure drying. Inspired by
limited dust releasing, aerogel powder was introduced to the PET
electrospinning solution in an attempt to create required bulk and
surface structure for the nanofibers to improve their hydrophobic and
insulation properties. The samples evaluation was carried out by
measuring density, porosity, contact angle, heat transfer, FTIR, BET,
and SEM. According to the results, porous silica aerogel powder was
fabricated with mean pore diameter of 24 nm and contact angle of
145.9º. The results indicated the usefulness of the aerogel powder
confined into nanofibers to control surface roughness for
manipulating superhydrophobic nanowebs with water contact angle
of 147º. It can be due to a multi-scale surface roughness which was
created by nanowebs structure itself and nanofibers surface
irregularity in presence of the aerogels while a layer of fluorocarbon
created low surface energy. The wettability of a solid substrate is an
important property that is controlled by both the chemical
composition and geometry of the surface. Also, a decreasing trend in
the heat transfer was observed from 22% for the nanofibers without
any aerogel powder to 8% for the nanofibers with 4% aerogel
powder. The development of thermal insulating materials has become
increasingly more important than ever in view of the fossil energy
depletion and global warming that call for more demanding energysaving
practices.
Abstract: Magnetic powder of Sr-ferrite was prepared by
conventional and sol-gel auto-combustion methods. In conventional
method, strontium carbonate and ferric oxide powders were mixed
together and then mixture was calcined. In sol-gel auto-combustion
method, a solution containing strontium nitrate, ferric nitrate and
citric acid was heated until the combustion took place automatically;
then, as-burnt powder was calcined. Thermal behavior, phase
identification, morphology and magnetic properties of powders
obtained by these two methods were compared by DTA, XRD, SEM
and VSM techniques. According to the results of DTA analysis,
formation temperature of Sr-ferrite obtained by conventional and solgel
auto-combustion methods were 1300°C and 1000°C, respectively.
XRD results confirmed the formation of pure Sr-ferrite at the
mentioned temperatures. Plate and hexagonal-shape particles of Srferrite
were observed using SEM. The Sr-ferrite powder obtained by
sol-gel auto-combustion method had saturation magnetization of
66.03 emu/g and coercivity of 5731 Oe in comparison with values of
58.20 emu/g and 4378 Oe obtained by conventional method.
Abstract: In the present study, we have synthesized Cr and Fe
doped zinc oxide (ZnO) nanostructures (Zn1-δCraFebO; where δ = a +
b = 20%, a = 5, 6, 8 & 10% and b = 15, 14, 12 & 10%) via sol-gel
method at different doping concentrations. The synthesized samples
were characterized for structural properties by X-ray diffractrometer
and field emission scanning electron microscope and the optical
properties were carried out through photoluminescence and UVvisible
spectroscopy. The particle size calculated through field
emission scanning electron microscope varies from 41 to 96 nm for
the samples synthesized at different doping concentrations. The
optical band gaps calculated through UV-visible spectroscopy are
found to be decreasing from 3.27 to 3.02 eV as the doping
concentration of Cr increases and Fe decreases.
Abstract: This article presents summary on preparation and
characterization of zinc, copper, cadmium and cobalt chromite
nanocrystals, embedded in an amorphous silica matrix. The
ZnCr2O4/SiO2, CuCr2O4/SiO2, CdCr2O4/SiO2 and CoCr2O4/SiO2
nanocomposites were prepared by a conventional sol-gel method
under acid catalysis. Final heat treatment of the samples was carried
out at temperatures in the range of 900−1200 ◦C to adjust the
phase composition and the crystallite size, respectively. The resulting
samples were characterized by Powder X-ray diffraction (PXRD),
High Resolution Transmission Electron Microscopy (HRTEM),
Raman/FTIR spectroscopy and magnetic measurements. Formation
of the spinel phase was confirmed in all samples. The average size of
the nanocrystals was determined from the PXRD data and by direct
particle size observation on HRTEM; both results were correlated.
The mean particle size (reviewed by HRTEM) was in the range from
∼4 to 46 nm. The results showed that the sol-gel method can be
effectively used for preparation of the spinel chromite nanoparticles
embedded in the silica matrix and the particle size is driven by the
type of the cation A2+ in the spinel structure and the temperature
of the final heat treatment. Magnetic properties of the nanocrystals
were found to be just moderately modified in comparison to the bulk
phases.
Abstract: In this paper, strontium ferrite (SrO.6Fe2O3) was
synthesized by the sol-gel auto-combustion process. The thermal
behavior of powder obtained from self-propagating combustion of
initial gel was evaluated by simultaneous differential thermal analysis
(DTA) and thermo gravimetric (TG), from room temperature to
1200°C. The as-burnt powder was calcined at various temperatures
from 700-900°C to achieve the single-phase Sr-ferrite. Phase
composition, morphology and magnetic properties were investigated
using X-ray diffraction (XRD), transmission electron microscopy
(TEM) and vibrating sample magnetometry (VSM) techniques.
Results showed that the single-phase and nano-sized hexagonal
strontium ferrite particles were formed at calcination temperature of
800°C with crystallite size of 27 nm and coercivity of 6238 Oe.
Abstract: The powders of Ba(Ce1-xZrx)0.90Y0.1O3-δ (BCZY) with 0.2 ≤ x ≤ 0.6 have been prepared by a modified sol-gel method. Triethylenetetramine (TETA) was employed as chelating agent. Phase formation of calcined powders at 1100oC and sintered pellets at 1400oC of BCZY were examined by an X-ray diffractrometer (XRD). XRD results showed the calcined powder and sintered pellet formed a single perovskite phase over the entire range of x values. As the amount of zirconium substitution (x values) increase, the main peaks are shifted to the higher 2theta values which suggest a complete substitution of zirconium into cerium sites. All the obtained calcined powders and sintered pellets possess cubic structure (Pm-3m) at all x values.
Abstract: Microfibrous palygorskite and tubular halloysite clay mineral combined with nanocrystalline TiO2 are incorporating in the preparation of nanocomposite films on glass substrates via sol-gel route at 450oC. The synthesis is employing nonionic surfactant molecule as pore directing agent along with acetic acid-based sol-gel route without addition of water molecules. Drying and thermal treatment of composite films ensure elimination of organic material lead to the formation of TiO2 nanoparticles homogeneously distributed on the palygorskite or halloysite surfaces. Nanocomposite films without cracks of active anatase crystal phase on palygorskite and halloysite surfaces are characterized by microscopy techniques, UV-Vis spectroscopy, and porosimetry methods in order to examine their structural properties.
The composite palygorskite-TiO2 and halloysite-TiO2 films with variable quantities of palygorskite and halloysite were tested as photocatalysts in the photo-oxidation of Basic Blue 41 azo dye in water. These nanocomposite films proved to be most promising photocatalysts and highly effective to dye’s decoloration in spite of small amount of palygorskite-TiO2 or halloysite-TiO2 catalyst immobilized onto glass substrates mainly due to the high surface area and uniform distribution of TiO2 on clay minerals avoiding aggregation.
Abstract: In this work, we have synthesized BaTiO3 via sol gel method by sintering at different temperatures (600, 700, 800, 900, 10000C) and studied their structural, optical and ferroelectric properties through X-ray diffraction (XRD), UV-Vis spectrophotometer and PE Loop Tracer. X-ray diffraction patterns of barium titanate samples show that the peaks of the diffractogram are successfully indexed with the tetragonal and cubic structure of BaTiO3. The Optical band gap calculated through UV Visible spectrophotometer varies from 4.37 to 3.80 eV for the samples sintered at 600 to 10000C, respectively. The particle size calculated through transmission electron microscopy varies from 20 to 40 nm for the samples sintered at 600 to 10000C, respectively. Moreover, it has been observed that the ferroelectricity increases as we increase the sintering temperature.