Effect of diethylene glycol content and annealing temperature on the structure and properties of poly(ethylene terephthalate)

The effect of 2,2′-oxydiethanol (diethylene glycol, DEG) content (ranging from 2 to 15 mol %) and of the annealing temperature (in the range from 100 to 260°C) on the density, calorimetric, dynamic- and static-mechanical and small angle X-ray scattering (SAXS) behavior of undrawn and drawn samples (granules, films, and bristles) of poly(ethylene terephthalate) (PET) has been studied. The known dependences on the annealing temperature are confirmed. Some discrepancies with earlier investigations of the dependences on the DEG content are established: constant values for the SAXS intensity and long spacing, for the lamellar thickness and for the volume fraction crystallinity a_c. These discrepancies are explained by the variation of the glass transition temperature (T_g) and melting temperature (T_m) of the materials with different DEG contents. The previous hypothesis of the segregation of the comonomer (DEG) units into the amorphous regions is confirmed.     

Crystal Structure of Ni5P2

It is shown by x-ray diffraction, energy-dispersive x-ray spectrometry, and electron probe microanalysis that, at 800°C, the Ni–P system contains four phosphides in the composition range 25–33 at % P: Ni₃P, Ni₅P₂, Ni₁₂P₅, and Ni₂P. The structure of Ni₅P₂ is determined by single-crystal x-ray diffraction: sp. gr. P3¯c1, new structure type, a = 0.6613(3) nm, c = 1.2311(6) nm, 347 independent hklreflections with F _hkl > 4(F _hkl), R _F = 0.0346. The key structural features of Ni₅P₂ are discussed.     

Direct electron microscopic observation of transcrystalline layers in microfibrillar reinforced polymer-polymer composites

Microfibrillar reinforced composites (MFC) comprising an isotropic matrix from a lower melting polymer, i.e., low density polyethylene (LDPE), reinforced by microfibrils of a higher melting polymer, recycled from bottles, i.e., poly(ethylene terephthalate) (PET), were processed under industrially relevant conditions via injection molding in a weight ratio of PET/LDPE = 50/50. Dog bone samples with MFC structure were characterized by means of scanning (SEM) and transmission (TEM) electron microscopy. SEM observations on cryogenic fracture surfaces show an isotropic LDPE matrix reinforced by more or less randomly distributed PET microfibrils. By means of TEM on stained ultrathin slices one observes the formation of transcrystalline layers of LDPE matrix on the surface of the PET microfibrils. In these layers the crystalline lamellae are aligned parallel to each other and are placed perpendicularly to the fibril surfaces. This is in contrast to the bulk matrix where the lamellae are quasi-randomly arranged.     

Finding a pipe's elastic and dimensional properties using ultrasonic guided wave cut-off frequencies

A non-destructive inverse procedure to determine a homogeneous, isotropic pipe's elastic properties and wall thickness is first described in principle. The procedure uses the cut-off frequencies of three ultrasonic guided wave modes that are employed with a semi-analytical finite element (SAFE) forward solver and the pipe's known density and outer diameter. Salient features of the computational process are illustrated by using forward and inverse numerical simulations. These simulations demonstrate that the cut-off frequencies need to be accurate. They can be found in practice from a short, unadulterated period of a response following the termination of an externally applied pulse. Then a direct temporal curve fitting technique is employed to improve the initial cut-off frequency estimates obtained from a discrete Fourier transform (DFT). A robust “nearest neighbour” search is used subsequently to simultaneously recover the elastic properties and wall thickness. Predicted nominal values are shown to agree well with corresponding values assigned in the computed forward solution. They are also confirmed using measurements of a physical pipe's dimensions and the experimental stress–strain behaviour from separately testing an off-cut.     

Effect of an obstacle during processing on the weld line of injection‐molded glassy polystyrene: Microhardness study

The microhardness (H) technique is used to characterize the quality of the weld line in injection‐molded glassy polystyrene by means of a cylindrical obstacle. In particular, the effect of the indentation location (closer or further from the obstacle edge parallel to the injection direction and across the weld line), both on the surface and in the bulk, was examined. Only for surface measurements close to the obstacle (up to 10 mm) a well‐pronounced decrease in H (～30%), followed by a sharp increase in a narrow distance (0.20–0.25 mm), was observed. For the bulk measurements on the same location a slight decrease in H was detected. Additional H measurements made up to 60 mm from the obstacle for both cases showed that the weld line remains undetectable. The results obtained reveal that the presence of a cylindrical obstacle causes the formation of a weld line on and near the surface only at distances not exceeding the obstacle diameter. At larger distances, because of the effective mutual interdiffusion of polymer chains, the two parallel fronts coming from the two sides of the obstacle developed a homogeneous material without any weld line according to the microhardness test. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 3362–3367, 2004     

Effect of blend composition on the morphology and mechanical properties of microfibrillar composites

Various blend compositions of polyethyleneterphthalate (PET) and polyamide 6 (PA 6) were used to prepare microfibrillar composites (MFC's) in form of thin ribbons. Steps for preparation were: (1) blending, (2) extrusion, (3) fibrillation, and (4) isotropization. The latter step was performed at a temperature condition above the melting temperature of PA 6, but below that of PET. In this way PET microfibrils remained as reinforcing elements in the PA 6-matrix. Depending on the actual PET/PA 6 ratio, various fibril arrangements in terms of fibril length and uniformity of fibril distribution could be achieved. A reasonable improvement in mechanical properties was reached already at 30 wt. % PET in PA 6 which was in terms of tensile strength higher than a 30 wt. % short glass fiber filled PA 6 system.     

Microhardness under strain. III. Microhardness behavior during stress-induced polymorphic transition in blends of poly(butylene terephthalate) and its block copolymers

The microhardness (H) technique was recently applied to poly(butylene terephthalate) (PBT) and its multiblock copolymer of poly(ether ester) (PEE) type for examination of the stress-induced polymorphic transition. In the present study, these investigations are extended to blends of PBT and PEE. For this purpose, drawn and annealed with fixed ends at 170°C for 6 h in vacuum bristles of PBT–PEE, blends were characterized with respect to their microhardness at various stages of tensile deformation. H was measured under stress, with each step of deformation amounting 5%. The variation of H with strain (ε) shows 2 sharp stepwise decreasing values (by 40%). Each step is defined in a relatively narrow deformation (ε) range (2–5%) due to the stress-induced α → β polymorphic transitions arising in PBT crystallites. The first polymorphic transition (at ε = 2–3%) is assigned to the PBT crystallites of the homopolymer (homoPBT). The second transition (at ε = 25%) is associated to those crystals within the PEE copolymer. From the observation of two distinct transitions, separated by a deformation interval of ε = 20% it is concluded that (1) homoPBT and the PBT segments from PEE crystallize separately (no cocrystallization takes place), and (2) the 2 species of PBT crystallites are subject to the external mechanical loading, not in a simultaneous manner, but in a two-stage process. In the deformation range between the 2 transitions (ε = 2–3% and 25%), it is pointed out that conformational changes are induced through stretching, mainly in the amorphous regions. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 69: 2271–2276, 1998