Authors:B. Rojas de Gáscue, J. Prin, D. Guerra, and C. Urbina de Navarro
This work presents a relationship between the thermal properties in different polyethylene samples analyzed by differential
scanning calorimetry (DSC). The morphology and structural changes were studied by transmission electron microscopy (TEM).
A preparative method involving surface etching was used to obtain surface replicas. The main morphological features of the
samples, characterized by lamellar structure, obtained in this work by TEM give values of mean lamellar thickness from 900
to 500 Ĺ in the highest branch content and molecular mass. Enthalpies of melting allowed to calculate crystallinity; given
values in the range from 47 to 68%.
Authors:S. Pagliolico, D. Marchisio, and A. Barresi
Precipitation of a sparingly soluble salt in the annular gap of a continuous Couette reactor with two unpremixed feeds has
been experimentally investigated. Barium chloride and sodium sulphate in stoichiometric ratio are fed at different flow rate
in the lower part of the reactor; different feeding modes have been considered. The dependence of precipitation yield, mean
crystal size and particle size distribution on rotation speed, axial flow rate and initial supersaturation ratio has been
studied. Depending on the operating conditions crystals with different morphologies have been obtained, varying from dentritic
tabular crystals to complex pyramidal ones and from single crystals to aggregates.
The DSC characterisation of the morphology of the metastable a phase of stoichiometric nickel sulphide was carried out using
two calorimeters; a TA Instruments 2920 MDSC and a Perkin Elmer DSC-7, and two quenching histories. Based on these quenching
histories, significant differences were observed in the heat flow curves, including the observation of a second exothermic
peak which is tentatively assigned to be a metastable phase to metastable phase transformation. The kinetic constants for
the a to b recrystallisation were determined as a function of degree of conversion using a mechanism free isoconversional
model. Variations in the values of the kinetic constants were also ascribed to the quenching histories. Although the differences
in morphology observed were ascribed to the processing history, the shift in the position of the a to b recrystallisation
peak was partially attributed to the thermal resistances of the instruments used.
Authors:B. Sauer, W. Kampert, R. McLean, and P. Carcia
The thermal and crystal morphological properties of poly[ethylene teraphthalate] (PET) and poly(ethylene-2,6-naphthalenedicarboxylate) (PEN) biaxially oriented films were compared to amorphous and other isotropic semi-crystalline samples. Crystal melting as a function of temperature was characterized by temperature modulated DSC (TMDSC) and found to begin just above the glass transition for both oriented films. About 75°C above the glass transitions, substantial exothermic recrystallization begins and continues through the final melting region in oriented films. The maximum in the non-reversing TMDSC signal for the oriented films signifies the maximum recrystallization exothermic activity with peaks at 248°C and 258°C for PET and PEN, respectively. The final melting endotherm detected was 260°C and 270°C for PET and PEN, and is shown by the TMDSC data and by independent rapid heating rate melting point determinations to be due to the melting of species recrystallized during the heating scan. The results are compared with TMDSC data for initially amorphous and melt crystallized samples. The volume fraction of rigid species (Frigid=total crystal fraction plus rigid amorphous or non-crystalline species) were measured by TMDSC glass transition data, and contrasted with the area fraction of rigid species at the oriented film surface characterized with very high resolution atomic force microscopy (AFM) phase data. The data suggest that the 11 nm wide hard domains in PET, and 21 nm wide domains in PEN film detected by AFM consist of both crystal and high stiffness interphase species.
Authors:R. Joshi, E. Lefevre, C. Patel, T. Provder, R. Crombez, W. Shen, and F. Jones
In the present report, thermal analysis (TMDSC, DMA, TG, stress-strain analysis), nano-indentation and AFM morphological characterization
of cross-linkable latexes, prepared with either a pre-coalescence cross-linker (1,3-butylene glycol dimethacrylate) or post-coalescence
cross-linker (adipic dihydrazide) at various levels of cross-linking, were done. The study assesses the effect of type and
level of cross-linking on the film formation process through the evolution of mechanical properties and latex morphology.
In addition, the final fundamental thermal and mechanical properties, specific end-use properties and latex morphology resulting
from the film formation process are reported.
Authors:C. Arribas, Rosa Masegosa, C. Salom, E. Arévalo, S. Prolongo, and Margarita Prolongo
Diglycidyl ether of bisfenol-A (DGEBA)/polybenzyl methacrylate (PBzMA)
blends cured with 4,4’-diaminodiphenylmethane (DDM) were studied. Miscibility,
phase separation, cure kinetics and morphology were investigated through differential
scanning calorimetry (DSC) and scanning electron microscopy (SEM). Non-reactive
DGEBA/PBzMA blends are miscible over the whole composition range. The addition
of PBzMA to the reactive (DGEBA+DDM) mixture slows down the curing rate, although
the reaction mechanism remains autocatalytic. On curing, initially miscible
(DGEBA+DDM)/PBzMA blends phase separate, arising two glass transition temperatures
that correspond to a PBzMA-rich phase and to epoxy network. Cured epoxy/PBzMA
blends present different morphologies as a function of the PBzMA content.
Authors:S. Mojumdar, J. Kozánková, J. Chocholoušek, J. Majling, and D. Fábryová
Fluoroapatite containing glass-ceramics were prepared from Li2O-CaO-CaF2-P2O5-SiO2 system. The glass was melted at 1480C for 1 h. The object of observation was the preparing crystal phase of fluoroapatite
in amorphous glass matrix. The morphology of lithium disilicate glass-ceramics was studied by SEM. The crystal growth and
thermal properties of fluoroapatite were studied by X-ray diffraction and DTA. The more the content of P2O5, the more the presence of fluoroapatite particles. SEM investigation clearly indicated the phase separation and formation
of a primary crystalline phase of fluoroapatite in the studied glass-ceramics. DTA curves of the fluoroapatite samples exhibit
exothermic effects in the temperature range 337-694C depending on the composition of the materials. The position of exothermic peak for lithium disilicate on DTA curves moves with increasing specific surfacetowards lower temperatures which points on its preferential surface crystallization. As far as physical qualities are concerned,
mainly color and gloss, the best qualities of all observed materials belong to glass-ceramics with 10% P2O5.
Authors:Margarita Prolongo, C. Arribas, Catalina Salom, and Rosa Masegosa
ether of bisfenol-A (DGEBA)/poly(vinyl acetate) (PVAc)/poly(4-vinyl phenol)
brominated (PVPhBr) ternary blends cured with 4,4’-diaminodiphenylmethane
(DDM) were investigated by differential scanning calorimetry (DSC), dynamic
mechanical thermal analysis (DMTA) and scanning electron microscopy (SEM).
Homogeneous (DGEBA+DDM)/PVPhBr networks with a unique Tg
are generated. Ternary blends (DGEBA+DDM)/PVAc/PVPhBr are initially miscible
and phase separate upon curing arising two Tgs
that correspond to a PVAc-rich phase and to epoxy network phase. Increasing
the PVPhBr content the Tgof
the PVAc phase move to higher temperatures as a consequence of the PVAc-PVPhBr
interactions. Different morphologies are generated as a function of the blend
Authors:M. Sánchez-Cabezudo, R. M. Masegosa, C. Salom, and M. G. Prolongo
order to improve their inherent brittleness. The initially miscible blend phase separates on curing to form a biphasic material. In these modified thermosets the morphology, which depends on the modifier content and curing conditions [ 1 ], is the main