Abstract: This study presents synthesis of novel block
copolymers of thienyl end capped ethoxylated nonyl phenol and
pyrrole via chemical oxidative polymerization. Ethoxylated nonyl
phenol (ENP) was reacted with 2-thiophenecarbonyl chloride in order
to synthesize a macromonomer containing thienyl end-group (ENPThC).
Then copolymers of ENP-ThC and pyrrole were synthesized
by chemical oxidative polymerization using iron (III) chloride as an
oxidant. ENP-ThC served both as a macromonomer and an emulsifier
for pyrrole with poor solubility in water.
The synthesized block copolymers (ENP-ThC-b-PPy) were
characterized by spectroscopic analysis and the electrical
conductivities were investigated with 4-point probe technique.
Abstract: The biosynthesis of nanoparticles by microorganisms,
on the contrary to chemical synthesis, is an environmentally-friendly
process which has low energy requirements. In this investigation, we
used the microorganism Geobacillus wiegelii, strain GWE1, an
aerobic thermophile belonging to genus Geobacillus, isolated from a
drying oven. This microorganism has the ability to reduce selenite
evidenced by the change of color from colorless to red in the culture.
Elemental analysis and composition of the particles were verified
using transmission electron microscopy and energy-dispersive X-ray
analysis. The nanoparticles have a defined spherical shape and a
selenium elemental state. Previous experiments showed that the
presence of the whole microorganism for the reduction of selenite
was not necessary. The results strongly suggested that an intracellular
NADPH/NADH-dependent reductase mediates selenium
nanoparticles synthesis under aerobic conditions. The enzyme was
purified and identified by mass spectroscopy MALDI-TOF TOF
technique. The enzyme is a 1-pyrroline-5-carboxylate dehydrogenase.
Histograms of nanoparticles sizes were obtained. Size distribution
ranged from 40-160 nm, where 70% of nanoparticles have less than
100 nm in size. Spectroscopic analysis showed that the nanoparticles
are composed of elemental selenium. To analyse the effect of pH in
size and morphology of nanoparticles, the synthesis of them was
carried out at different pHs (4.0, 5.0, 6.0, 7.0, 8.0). For
thermostability studies samples were incubated at different
temperatures (60, 80 and 100 ºC) for 1 h and 3 h. The size of all
nanoparticles was less than 100 nm at pH 4.0; over 50% of
nanoparticles have less than 100 nm at pH 5.0; at pH 6.0 and 8.0 over
90% of nanoparticles have less than 100 nm in size. At neutral pH
(7.0) nanoparticles reach a size around 120 nm and only 20% of them
were less than 100 nm. When looking at temperature effect,
nanoparticles did not show a significant difference in size when they
were incubated between 0 and 3 h at 60 ºC. Meanwhile at 80 °C the
nanoparticles suspension lost its homogeneity. A change in size was
observed from 0 h of incubation at 80ºC, observing a size range
between 40-160 nm, with 20% of them over 100 nm. Meanwhile
after 3 h of incubation at size range changed to 60-180 nm with 50%
of them over 100 nm. At 100 °C the nanoparticles aggregate forming
nanorod structures. In conclusion, these results indicate that is
possible to modulate size and shape of biologically synthesized
nanoparticles by modulating pH and temperature.
Abstract: Three dimensional non-Interlaced carbon fibre
reinforced silicon carbide (3-D-Cf/SiC) composites with pyrocarbon
interphase were fabricated using isothermal chemical vapor
infiltration (ICVI) combined with polymer impregnation pyrolysis
(PIP) process. Polysilazane (PSZ) is used as a preceramic polymer to
obtain silicon carbide matrix. Thermo gravimetric analysis (TGA),
Infrared spectroscopic analysis (IR) and X-ray diffraction (XRD)
analysis were carried out on PSZ pyrolysed at different temperatures
to understand the pyrolysis and obtaining the optimum pyrolysing
condition to yield β-SiC phase. The density of the composites was
1.94 g cm-3 after the 3-D carbon preform was SiC infiltrated for 280 h
with one intermediate polysilazane pre-ceramic PIP process.
Mechanical properties of the composite materials were investigated
under tensile, flexural, shear and impact loading. The values of
tensile strength were 200 MPa at room temperature (RT) and 195
MPa at 500°C in air. The average RT flexural strength was 243 MPa.
The lower flexural strength of these composites is because of the
porosity. The fracture toughness obtained from single edge notched
beam (SENB) technique was 39 MPa.m1/2. The work of fracture
obtained from the load-displacement curve of SENB test was 22.8
kJ.m-2. The composites exhibited excellent impact resistance and the
dynamic fracture toughness of 44.8 kJ.m-2 is achieved as determined
from instrumented Charpy impact test. The shear strength of the
composite was 93 MPa, which is significantly higher compared 2-D
Cf/SiC composites. Microstructure evaluation of fracture surfaces
revealed the signatures of fracture processes and showed good
support for the higher toughness obtained.
Abstract: Theoretical investigations are performed by DFT method of B3LYP/6-31G+(2d,p) and B3LYP/6-311G+(2d,p) basis sets for three carbonyl thiourea compounds, namely N-[(2,6-Diethylphenyl)carbamothioyl]-2,2-diphenylacetamide (Compound I), N-[(3-Ethylphenyl)carbamothioyl]-2,2-diphenylacetamide (Compound II) and 2,2-Diphenyl-N-{[2-(trifluoromethyl)phenyl]carbamothioyl}acetamide (Compound III). Theoretical calculations for bond parameters, harmonic vibration frequencies and isotropic chemical shifts are in good agreement with the experimental results. The calculated molecular vibrations show good correlation values, which are 0.998 and 0.999 with the experimental data. The energy gap for compounds I, II and III calculated at B3LYP/6-31G+(2d,p) basis set are 4.455866117, 4.297495791 and 4.313550514 eV respectively, while for B3LYP/6-311G+(2d,p) basis set the energy gap obtained are 4.453689205 (Compound I), 4.311373603 (Compound II) and 4.315727426 (Compound III) eV.
Abstract: The research study was based on an evaluation of the
ability of glued test samples to pass the criterion of sufficient
bondline adhesion under the exposure conditions defined in EN 302-
1. Additionally, an infrared spectroscopic analysis of the evaluated
adhesives (phenol-resorcinol-formaldehyde PRF and melamine-ureaformaldehyde
MUF) with different mix ratios was carried out to
evaluate the possible effects of a faulty technological process.