Abstract: The irradiation of polymeric materials has received
much attention because it can produce diverse changes in chemical
structure and physical properties. Thus, studying the chemical and
structural changes of polymers is important in practice to achieve
optimal conditions for the modification of polymers. The effect of
gamma irradiation on the crystalline structure of poly(vinylidene
fluoride) (PVDF) has been investigated using differential scanning
calorimetry (DSC) and X-ray diffraction techniques (XRD). Gamma
irradiation was carried out in atmosphere air with doses between 100
kGy at 3,000 kGy with a Co-60 source. In the melting thermogram of
the samples irradiated can be seen a bimodal melting endotherm is
detected with two melting temperature. The lower melting
temperature is attributed to melting of crystals originally present and
the higher melting peak due to melting of crystals reorganized upon
heat treatment. These results are consistent with those obtained by
XRD technique showing increasing crystallinity with increasing
irradiation dose, although the melting latent heat is decreasing.
Abstract: This paper presents the effects of mixing procedures
on mechanical properties of flyash-based geopolymer matrices
containing nanosilica (NS) at 0.5%, 1.0%, 2.0%, and 3.0% by weight.
Comparison is made with conventional mechanical dry-mixing of NS
with flyash and wet-mixing of NS in alkaline solutions. Physical and
mechanical properties are investigated using X-Ray Diffraction
(XRD) and Scanning Electron Microscope (SEM). Results show that
generally the addition of NS particles enhanced the microstructure
and improved flexural and compressive strengths of geopolymer
nanocomposites. However, samples, prepared using dry-mixing
approach, demonstrate better physical and mechanical properties
comparing to wet-mixing samples.
Abstract: Online measurement of the product quality is a
challenging task in cement production, especially in the production of
Celitement, a novel environmentally friendly hydraulic binder. The
mineralogy and chemical composition of clinker in ordinary Portland
cement production is measured by X-ray diffraction (XRD) and
X-ray fluorescence (XRF), where only crystalline constituents can be
detected. But only a small part of the Celitement components can be
measured via XRD, because most constituents have an amorphous
structure. This paper describes the development of algorithms
suitable for an on-line monitoring of the final processing step of
Celitement based on NIR-data. For calibration intermediate products
were dried at different temperatures and ground for variable
durations. The products were analyzed using XRD and
thermogravimetric analyses together with NIR-spectroscopy to
investigate the dependency between the drying and the milling
processes on one and the NIR-signal on the other side. As a result,
different characteristic parameters have been defined. A short
overview of the Celitement process and the challenging tasks of the
online measurement and evaluation of the product quality will be
presented. Subsequently, methods for systematic development of
near-infrared calibration models and the determination of the final
calibration model will be introduced. The application of the model on
experimental data illustrates that NIR-spectroscopy allows for a quick
and sufficiently exact determination of crucial process parameters.
Abstract: Cadmium oxide (CdO) nanoparticles have been
prepared by chemical coprecipitation method. The synthesized
nanoparticles were characterized by X-ray diffraction analysis
(XRD), scanning electron microscopy (SEM), transmission electron
microscopy (TEM), UV analysis, and dielectric studies. The
crystalline nature and particle size of the CdO nanoparticles were
characterized by Powder X-ray diffraction analysis (XRD). The
morphology of prepared CdO nanoparticles was studied by scanning
electron microscopy. The particle size was studied using the
transmission electron microscopy (TEM).The optical properties were
obtained from UV-Vis absorption spectrum. The dielectric properties
of CdO nanoparticles were studied in the frequency range of 50 Hz–5
MHz at different temperatures. The frequency dependence of the
dielectric constant and dielectric loss is found to decrease with an
increase in the frequency at different temperatures. The ac
conductivity of CdO nanoparticle has been studied.
Abstract: Geopolymer composites reinforced with flax fabrics
and nanoclay are fabricated and studied for physical and mechanical
properties using X-Ray Diffraction (XRD), Fourier Transform
Infrared Spectroscopy (FTIR), and Scanning Electron Microscope
(SEM). Nanoclay platelets at a weight of 1.0%, 2.0%, and 3.0% were
added to geopolymer pastes. Nanoclay at 2.0 wt.% was found to
improve density and decrease porosity while improving flexural
strength and post-peak toughness. A microstructural analysis
indicated that nanoclay behaves as filler and as an activator
supporting geopolymeric reaction while producing a higher content
geopolymer gel improving the microstructure of binders. The process
enhances adhesion between the geopolymer matrix and flax fibres.
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: The 1:1 cocrystal of 2-amino-4-chloro-6-
methylpyrimidine (2A4C6MP) with 4-methylbenzoic acid (4MBA)
(I) has been prepared by slow evaporation method in methanol,
which was crystallized in monoclinic C2/c space group, Z = 8, and a
= 28.431 (2) Å, b = 7.3098 (5) Å, c = 14.2622 (10) Å and β =
109.618 (3)°. The presence of unionized –COOH functional group in
cocrystal I was identified both by spectral methods (1H and 13C
NMR, FTIR) and X-ray diffraction structural analysis. The
2A4C6MP molecule interact with the carboxylic group of the
respective 4MBA molecule through N—H⋯O and O—H⋯N
hydrogen bonds, forming a cyclic hydrogen–bonded motif R2
2(8).
The crystal structure was stabilized by Npyrimidine—H⋯O=C and
C=O—H⋯Npyrimidine types hydrogen bonding interactions.
Theoretical investigations have been computed by HF and density
function (B3LYP) method with 6–311+G (d,p)basis set. The
vibrational frequencies together with 1H and 13C NMR chemical
shifts have been calculated on the fully optimized geometry of
cocrystal I. Theoretical calculations are in good agreement with the
experimental results. Solvent–free formation of this cocrystal I is
confirmed by powder X-ray diffraction analysis.
Abstract: Within this paper, latest results on processing of energetic nanomaterials by means of the Spray Flash Evaporation technique are presented. This technology constitutes a highly effective and continuous way to prepare fascinating materials on the nano- and micro-scale. Within the process, a solution is set under high pressure and sprayed into an evacuated atomization chamber. Subsequent ultrafast evaporation of the solvent leads to an aerosol stream, which is separated by cyclones or filters. No drying gas is required, so the present technique should not be confused with spray dying. Resulting nanothermites, insensitive explosives or propellants and compositions are foreseen to replace toxic (according to REACH) and very sensitive matter in military and civil applications. Diverse examples are given in detail: nano-RDX (n-Cyclotrimethylentrinitramin) and nano-aluminum based systems, mixtures (n-RDX/n-TNT - trinitrotoluene) or even cocrystalline matter like n-CL-20/HMX (Hexanitrohexaazaisowurtzitane/ Cyclotetra-methylentetranitramin). These nanomaterials show reduced sensitivity by trend without losing effectiveness and performance. An analytical study for material characterization was performed by using Atomic Force Microscopy, X-Ray Diffraction, and combined techniques as well as spectroscopic methods. As a matter of course, sensitivity tests regarding electrostatic discharge, impact, and friction are provided.
Abstract: NiFe2O4 (nickel ferrite), ZnFe2O4 (zinc ferrite) and
Ni0.5Zn0.5Fe2O4 (nickel-zinc ferrite) were prepared by
mechanochemical route in a planetary ball mill starting from mixture
of the appropriate quantities of the Ni(OH)2/Fe(OH)3,
Zn(OH)2/Fe(OH)3 and Ni(OH)2/Zn(OH)2/Fe(OH)3 hydroxide
powders. In order to monitor the progress of chemical reaction and
confirm phase formation, powder samples obtained after 25 h, 18 h
and 10 h of milling were characterized by X-ray diffraction (XRD),
transmission electron microscopy (TEM), IR, Raman and Mössbauer
spectroscopy. It is shown that the soft mechanochemical method, i.e.
mechanochemical activation of hydroxides, produces high quality
single phase ferrite samples in much more efficient way. From the IR
spectroscopy of single phase samples it is obvious that energy of
modes depends on the ratio of cations. It is obvious that all samples
have more than 5 Raman active modes predicted by group theory in
the normal spinel structure. Deconvolution of measured spectra
allows one to conclude that all complex bands in the spectra are made
of individual peaks with the intensities that vary from spectrum to
spectrum. The deconvolution of Raman spectra allows to separate
contributions of different cations to a particular type of vibration and
to estimate the degree of inversion.
Abstract: Cesium molybdates with general formula
CsMIII(MoO4)2, where MIII = Bi, Dy, Pr, Er, exhibit rich
polymorphism, and crystallize in a layered structure. These properties
cause intensive studies on cesium molybdates. CsBi(MoO4)2 was synthesized by microwave method by using
cerium sulphate, bismuth oxide and molybdenum (VI) oxide in an
appropriate molar ratio. Characterizations were done by x-ray
diffraction (XRD), fourier transform infrared (FTIR) spectroscopy,
scanning electron microscopy/energy dispersive analyze (SEM/EDS),
thermo gravimetric/differantial thermal analysis (TG/DTA).
Abstract: The present study deals with the characterization of
CrSiN coatings obtained by PVD magnetron sputtering systems.
CrSiN films were deposited with different Si contents, in order to
check the effect of at.% variation on the different properties of the
Cr–N system. Coatings were characterized by scanning electron
microscopy (SEM) for thickness measurements, X-ray diffraction.
Surface morphology and the roughness characteristics were explored
using AFM, Mechanicals properties, elastic and plastic deformation
resistance of thin films were investigated using nanoindentation test. We observed that the Si addition improved the hardness and the
Young’s modulus of the Cr–N system. Indeed, the hardness value is
18,56 GPa for CrSiN coatings. Besides, the Young’s modulus value
is 224,22 GPa for CrSiN coatings for Si content of 1.2 at.%.
Abstract: The ferrites ZnFe2O4, CdFe2O4 and CuFe2O4 are
synthesized in laboratory conditions using ceramic technology. Their
homogeneity and structure are proven by X-Ray diffraction analysis
and Mössbauer spectroscopy. The synthesized ferrites are subjected
to strong acid and high temperature leaching with solutions of H2SO4,
HCl and HNO3. The results indicate that the highest degree of
leaching of Zn, Cd and Cu from the ferrites is achieved by use of
HCl. The charging of five zinc sulfide concentrates was optimized using
the criterion of minimal amount of zinc ferrite produced when
roasting the concentrates in a fluidized bed. The results obtained are
interpreted in terms of the hydrometallurgical zinc production and
maximum recovery of zinc, copper and cadmium from initial zinc
concentrates after their roasting.
Abstract: Zinc borate is an important inorganic hydrate borate
material, which can be used as a flame retardant agent and corrosion
resistance material. This compound can loss its structural water
content at higher than 290°C. Due to thermal stability; Zinc Borate
can be used as flame retardant at high temperature process of plastic
and gum. In this study, the ultrasonic reaction of zinc borates were
studied using hydrozincite (Zn5(CO3)2·(OH)6) and boric acid
(H3BO3) raw materials. Before the synthesis raw materials were
characterized by X-Ray Diffraction (XRD) and Fourier Transform
Infrared Spectroscopy (FT-IR). Ultrasonic method is a new
application on the zinc borate synthesis. The synthesis parameters
were set to 90°C reaction temperature and 55 minutes of reaction
time, with 1:1, 1:2, 1:3, 1:4 and 1:5 molar ratio of starting materials
(Zn5(CO3)2·(OH)6 : H3BO3). After the zinc borate synthesis, the
products were analyzed by XRD and FT-IR. As a result, optimum
molar ratio of 1:5 is determined for the synthesis of zinc borates with
ultrasonic method.
Abstract: Natural fibers are used in polymer composites to
improve mechanical properties to replace inorganic reinforcing
agents produced by non-renewable resources. The present study
investigates the tensile and flexural behaviors of palm fibers-high
density polyethylene (HDPE) composite as a function of volume
fraction. The surface of the fibers was treated by mercerization
treatments to improve the wetting behavior of the apolar HDPE. The
treatment characterization was obtained by scanning electron
microscopy, X-Ray diffraction and infrared spectroscopy. Results
evidences that a good adhesion interfacial between fibers-matrix
caused an increase strength and modulus flexural as well as tensile
strength in the modified fibers/HDPE composites when compared to
the pure HDPE and untreated fibers reinforced composites.
Abstract: Calcium Phosphate Cement (CPC) due to its high bioactivity and optimum bioresorbability shows excellent bone regeneration capability. Despite it has limited applications as bone implant due to its macro-porous microstructure causing its poor mechanical strength. The reinforcement of apatitic CPCs with biocompatible fibre glass phase is an attractive area of research to improve upon its mechanical strength. Here, we study the setting behaviour of Si-doped and un-doped α tri calcium phosphate (α - TCP) based CPC and its reinforcement with addition of E-glass fibre. Alpha Tri calcium phosphate powders were prepared by solid state sintering of CaCO3 , CaHPO4 and Tetra Ethyl Ortho Silicate (TEOS) was used as silicon source to synthesize Si doped α-TCP powders. Both initial and final setting time of the developed cement was delayed because of Si addition. Crystalline phases of HA (JCPDS 9- 432), α-TCP (JCPDS 29-359) and β-TCP (JCPDS 9-169) were detected in the X-ray diffraction (XRD) pattern after immersion of CPC in simulated body fluid (SBF) for 0 hours to 10 days. As Si incorporation in the crystal lattice stabilized the TCP phase, Si doped CPC showed little slower rate of conversion into HA phase as compared to un-doped CPC. The SEM image of the microstructure of hardened CPC showed lower grain size of HA in un-doped CPC because of premature setting and faster hydrolysis of un-doped CPC in SBF as compared that in Si-doped CPC. Premature setting caused generation of micro and macro porosity in un-doped CPC structure which resulted in its lower mechanical strength as compared to that in Si-doped CPC. It was found that addition of 10 wt% of E-glass fibre into Si-doped α-TCP increased the average DTS of CPC from 8 MPa to 15 MPa as the fibres could resists the propagation of crack by deflecting the crack tip. Our study shows that biocompatible E-glass fibre in optimum proportion in CPC matrix can enhance the mechanical strength of CPC without affecting its biocompatibility.
Abstract: The first laboratory synthesis of hard materials such as
diamond proceeded to attack of developing materials with high
hardness to compete diamond. Boron rich solids are good candidates
owing to their short interatomic bond lengths and strong covalent
character. Boron containing hard material was synthesized by modifiedmicrowave
method under nitrogen atmosphere by using a fuel
(glycine or urea), amorphous boron and/or boric acid in appropriate
molar ratio. Characterizations were done by x-ray diffraction (XRD),
Fourier transform infrared (FTIR) spectroscopy, scanning electron
microscopy/energy dispersive analyze (SEM/EDS), thermo
gravimetric/differential thermal analysis (TG/DTA).
Abstract: The aim of this study was to investigate the
photocatalytic activity of polycrystalline phases of bismuth tungstate
of formula Bi2WO6. Polycrystalline samples were elaborated using a
coprecipitation technique followed by a calcination process at
different temperatures (300, 400, 600 and 900°C). The obtained
polycrystalline phases have been characterized by X-ray diffraction
(XRD), scanning electron microscopy (SEM), and transmission
electron microscopy (TEM). Crystal cell parameters and cell volume
depend on elaboration temperature. High-resolution electron
microscopy images and image simulations, associated with X-ray
diffraction data, allowed confirming the lattices and space groups
Pca21. The photocatalytic activity of the as-prepared samples was
studied by irradiating aqueous solutions of Rhodamine B, associated
with Bi2WO6 additives having variable crystallite sizes. The
photocatalytic activity of such bismuth tungstates increased as the
crystallite sizes decreased. The high specific area of the
photocatalytic particles obtained at 300°C seems to condition the
degradation kinetics of RhB.
Abstract: The effect of carbon nanofibers (CNFs) on the
electrical properties of Poly(vinylidene fluoride-hexafluoropropylene)
(P(VdF-HFP)) based gel polymer electrolytes has been investigated
in the present work. The length and diameter ranges of CNFs used in
the present work are 5-50 μm and 200-600 nm respectively. The
nanocomposite gel polymer electrolytes have been synthesized by
solution casting technique with varying CNFs content in terms of
weight percentage. Electrochemical impedance analysis demonstrates
that the reinforcement of carbon nanofibers significantly enhances the
ionic conductivity of the polymer electrolyte. The decrease of
crystallinity of P(VdF-HFP) due the addition of CNFs has been
confirmed by X-ray diffraction (XRD). The interaction of CNFs with
various constituents of nanocomposite gel polymer electrolytes has
been assessed by Fourier Transform Infrared (FTIR) spectroscopy.
Moreover CNFs added gel polymer electrolytes offer superior
thermal stability as compared to that of CNFs free electrolytes as
confirmed by Thermogravimetric analysis (TGA).
Abstract: In this paper, we study the optical nonlinearities of
Silver sulfide (Ag2S) nanostructures dispersed in the Dimethyl
sulfoxide (DMSO) under exposure to 532 nm, 15 nanosecond (ns)
pulsed laser irradiation. Ultraviolet–visible absorption spectrometry
(UV-Vis), X-ray diffraction (XRD), and transmission electron
microscopy (TEM) are used to characterize the obtained nanocrystal
samples. The band gap energy of colloid is determined by analyzing
the UV–Vis absorption spectra of the Ag2S NPs using the band
theory of semiconductors. Z-scan technique is used to characterize
the optical nonlinear properties of the Ag2S nanoparticles (NPs).
Large enhancement of two photon absorption effect is observed with
increase in concentration of the Ag2S nanoparticles using open Zscan
measurements in the ns laser regime. The values of the nonlinear
absorption coefficients are determined based on the local nonlinear
responses including two photon absorption. The observed aperture
dependence of the Ag2S NP limiting performance indicates that the
nonlinear scattering plays an important role in the limiting action of
the sample. The concentration dependence of the optical liming is
also investigated. Our results demonstrate that the optical limiting
threshold decreases with increasing the silver sulfide NPs in DMSO.
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.