Differential scanning calorimetry (DSC) is one of the most widely used technique for measuring crystallinity in the polymer industry. The major source of error in the crystalline index (CIDSC) of low crystallinity polymeric articles, is the development of further crystallinity during the DSC scan. Although, this type of cold crystallization is obvious, and thus accounted for in polymers like polyethylene terephthalate, nylons are a difficult class of materials in that respect. The major contributing factors to the failure of DSC in measuring low levels of crystallinity in nylons are identified to be (1) silent crystallization between the glass (Tg) and melting (Tm) transitions, (2) extreme difficulties in packing a moisture‐free nylon in the sample pan (the response due to traces of moisture being a broad endotherm competing with a broad exothermic crystallization), and (3) a sub‐Tm exotherm, especially in low crystallinity nylons, due to relaxation of the processing‐induced stresses. These factors, specific to nylons, mask the observation of cold crystallization and lead to substantially higher than real crystallinities. This manuscript deals with such complications and corrective actions using commercial nylon 6 films of CIDSC = 0−40%. X‐ray diffraction measurements have been included to support the validity of our improved DSC methodology. © 1997 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 35: 2219–2231, 1997
Although it has long been known that the glass transition temperature (T,) of nylons changes significantly with moisture content, literature to date has lacked reliable measurements of this type, primarily due to the changes in moisture during the Tg scanning experiments. Introduction of the new dynamic DSC technique has allowed us to quantify the dependence of Tg on % relative humidity for nylon 6 and nylon 66. By eliminating the possibility of moisture pickup, we have been able to separate the effect of crystallinity as well as orientation on the Tg of nylon 6. The methodology described here should be applicable to other moisture sensitive polymers as well, e.g., poly(viny1 alcohol).
The optical aberrations induced by imaging through skin can be predicted using formulas for Seidel aberrations of a plane-parallel plate. Knowledge of these aberrations helps to guide the choice of numerical aperture (NA) of the optics we can use in an implementation of Gabor domain optical coherence microscopy (GD-OCM), where the focus is the only aberration adjustment made through depth. On this basis, a custom-designed, liquid-lens enabled dynamic focusing optical coherence microscope operating at 0.2 NA is analyzed and validated experimentally. As part of the analysis, we show that the full width at half-maximum metric, as a characteristic descriptor for the point spread function, while commonly used, is not a useful metric for quantifying resolution in non-diffraction-limited systems. Modulation transfer function (MTF) measurements quantify that the liquid lens performance is as predicted by design, even when accounting for the effect of gravity. MTF measurements in a skinlike scattering medium also quantify the performance of the microscope in its potential applications. To guide the fusion of images across the various focus positions of the microscope, as required in GD-OCM, we present depth of focus measurements that can be used to determine the effective number of focusing zones required for a given goal resolution. Subcellular resolution in an onion sample, and high-definition in vivo imaging in human skin are demonstrated with the custom-designed and built microscope.
Physical blends of nylon 6 (or nylon 66) homopolymer with random copolymers of nylon 6/nylon 66 or of nylon 6/nylon 12 were melt extruded into films and characterized by Differential Scanning Calorimetry (DSC) and X‐ray Diffraction (XRD) techniques. The films containing up to 50–65% of the copolymer exhibited only a single melting temperature (Tm) corresponding to that of the pure homopolymer without any trace of the otherwise crystallizable, lower melting copolymer component. These observations are quite unusual since the binary blends of the homopolymers of nylon 6, nylon 66, and nylon 12 exhibit their characteristic 2 Tm's. That result was significant in that at least 20% nylon 6 units (Tm = 222°C) can be incorporated into nylon 66 (Tm = 262°C) without any depression either in the Tm or in the crystallinity of nylon 66 while retaining its Tm = 262°C as the only melting phase. Also, it has now become possible to develop blend compositions based on ≥ 4 polyamide moieties that exhibit a single Tg, high crystallinity, and a sigle Tm corresponding to the higest melting component. We believe that the observed phenomenon, pseudo super‐miscibility, is kinetically driven (i.e., only the higher melting homopolymer crystallizes), rather than thermodynamically or crystallographically, since the structural units originate from polymers that are inherently not isomorphic. In view of the unexpected observation, at least in the field of nylons and its technological significance, we anticipate renewed interest in this area and more definitive understanding to emerge from future studies.
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