Authors:L. Torre, J. Kenny, A. Recca, V. Siracusa, A. Tarzia, and A. Maffezzoli
An analysis of the crystallization behaviour of a new poly(aryl-ether-ether-ketone-ketone), PK99, by differential scanning
calorimetry (DSC) and wide-angle X-ray diffraction (WAXD) is presented. Isothermal crystallization TG were obtained in the
whole range between the glass transition temperature (Tg) and the melting temperature (Tm) as a consequence of the slow crystallization kinetics stemming from the closeness of these transitions. The calorimetric
results, compared with WAXD data, were applied to determine the theoretical melting temperature and crystallization enthalpy.
The DSC and WAXD data were combined in order to calculate the total amount of the crystallizable fraction of the polymer,
and a model was proposed to explain the difference between the fractions of crystallinity observed with these techniques.
The thermal and X-ray data were also correlated with different lamellar morphologies arising from the crystallization conditions.
Finally, DSC experiments on the crystallized sample were used to detect the presence of a rigid amorphous phase which does
not relax at Tg.
Composites of poly(vinyl pyrrolidone)/hydroxyapatite (PVP/HA), at variable proportions (100/0; 80/20; 50/50; 20/80 wt%) were
prepared and characterized by Fourier transformer-infrared spectroscopy (FT-IR), wide angle X-ray diffraction (WAXD), differential
scanning calorimetry (DSC), and thermogravimetry/differential thermogravimetry (TG/DTG). PVP carbonyl stretching was slightly
shifted to lower frequency in composites indicating the formation of hydrogen bonding with HA hydroxyl groups. At the first
cycle of heating, the calorimetric curves revealed a broad peak the intensity of which was reduced insofar as the amount of
PVP decreased in the composites. This peak was attributed to the PVP enthalpy relaxation. According to the TG/DTG curves,
PVP degraded into two steps sharply perceivable in the composites. The first decay was ascribed to the release of the pyrrolidone
pendant groups and the following one concerned the burning of the hydrocarbon chains. The HA molecules seem to exert a catalytic
action on the PVP degradation.
Authors:W. Liu, S. Kim, J. Lopez, B. Hsiao, M. Keating, I.-H. Lee, B. Landes, and R. Stein
In this study, the stepwise isothermal crystallization or thermal fractionation of Ziegler—Natta and metallocene based polyethylenes (ZN-PE and m-PE) with two kinds of branch lengths (ethyl and hexyl) and branch compositions were studied using simultaneous synchrotron small-angle X-ray scattering (SAXS)/wide-angle X-ray diffraction (WAXD) and differential scanning calorimetry (DSC). The crystal long period and the invariant were determined by SAXS, and the variations of crystal unit cell parameters and the degree of crystallinity were determined by WAXD. The arithmetic mean length (Ln), the weightedmean length (Lw) and the broadness index (Lw/Ln) of the studied polyethylenes were previously determined by DSC. Results from these studies were interpreted using the model of branch exclusion, which affects the ability of the chain-reentry into the crystal phase. Multiple SAXS peaks and step-change in crystallinity change (WAXD) were seen during heating, which corresponded well with the crystal thickness distribution induced by stepwise crystallization. The effects of the heterogeneity of the 1-olefin branch length and the distribution on the crystal long period and the invariant as well as the degree of crystallinity were discussed.
Authors:V. Causin, Carla Marega, Roberta Saini, A. Marigo, and G. Ferrara
The effect of clay dispersion on the crystallization behavior of isotactic polypropylene (iPP)-based nanocomposites is reported.
The Tm0 of the materials was calculated by the method proposed by Marand, the kinetics of crystallization was evaluated by the Avrami
analysis and also the Hoffman-Lauritzen theory of crystallization regimes was applied. Montmorillonite was found to depress
Tm0, to enhance the rate of crystallization and to ease the chain folding of macromolecules. These effects were magnified if
clay was exfoliated, rather than intercalated.
Authors:H. Starkweather, P. Avakian, K. Gardner, B. Hsiao, M. Keating, and H. Ng
The polyamide from 2-methylpentamethylenediamine and dodecanedioic acid (MPMD-12) has been studied by differential scanning calorimetry, dynamic mechanical analysis, dielectric analysis, X-ray crystallography, and simultaneous small and wide-angle X-ray scattering using synchrotron radiation. The polymer exhibits polymorphism which is shown to be associated with the incorporation of the branched diamine. At relatively low temperatures, the crystal structure is similar to the gamma form which has been found in many other polyamides. At higher temperatures, a new delta form appears in which the diamine moiety adopts a bent conformation. In this form, the chains follow a zig-zag pattern with two chemical repeats units per crystallographic repeat with a shortening of about 10% along the c-axis.
Authors:Zhen Li, Li Yu, Liqiang Zheng, and Fei Geng
SLN, nanoparticles loaded with or without puerarin. The crystalline states of these two kinds of SLN were studied by DSC and WAXD. In addition to this, the crystallization states of SLN prepared by the method of double emulsion and microemulsion were
Authors:Shinn-Gwo Hong, Tsung-Kai Gau, and Shih-Che Huang
The WAXD patterns of the representative specimens are also shown in Fig. 5 and from which the effects of added modifiers on PHB crystal structures can be obtained. As seen, the basic WAXD patterns from the α-form crystals of PHB are observed in all
Authors:A. V. Maldhure, A. R. Chaudhari, and Jayant D. Ekhe
shows the WAXD pattern of PPML blends which indicated that the neat PP in blends crystallizes primarily in monoclinic α-form via reflections at 2θ of 14.1, 16.8, 18.5, 21.1, and 22.0 corresponding to 110, 040, 130, 111, and 041 planes and exhibits the β
Wide angle X-ray diffraction (WAXD)
The crystalline structure was determined by WAXD analysis. The specimens for WAXD were prepared by compression molding into 1-mm-thick sheets at 200 °C. WAXD profiles were recorded on a PANalytical X