Differential scanning calorimetry amorphous polymers

A variety of techniques have been used to determine the extent of crystallinity in a polymer, including X-ray diffraction, density, IR, NMR, and heat of fusion [Sperling, 2001 Wunderlich, 1973], X-ray diffraction is the most direct method but requires the somewhat difficult separation of the crystalline and amorphous scattering envelops. The other methods are indirect methods but are easier to use since one need not be an expert in the field as with X-ray diffraction. Heat of fusion is probably the most often used method since reliable thermal analysis instruments are commercially available and easy to use [Bershtein and Egorov, 1994 Wendlandt, 1986], The difficulty in using thermal analysis (differential scanning calorimetry and differential thermal analysis) or any of the indirect methods is the uncertainty in the values of the quantity measured (e.g., the heat of fusion per gram of sample or density) for 0 and 100% crystalline samples since such samples seldom exist. The best technique is to calibrate the method with samples whose crystallinites have been determined by X-ray diffraction. 

Various methods have been employed to find out about the structure of polymer electrolytes. These include thermal methods such as differential scanning calorimetry (DSC), differential thermal analysis (DTA), X-ray methods such as X-ray diffraction and X-ray absorption fine structure (XAFS), solid state NMR methods particularlyusing7LiNMR,andvibrationalspectroscopicmethodssuch as infrared and Raman [27]. The objective of these various studies is to establish the structural identity of the polymer electrolyte at the macroscopic as well as the molecular levels. Thus the points of interest are the crystallinity or the amorphous nature of materials, the glass transition temperatures, the nature and extent of interaction between the added metal ion and the polymer, the formation of ion pairs etc. Ultimately the objective is to understand how the structure (macroscopic and molecular) of the polymer electrolyte is related to its behavior particularly in terms of ionic conductivity. Most of the studies have been carried out, quite understandably, on PEO-metal salt complexes. In comparison, there has been no attention on the structural aspects of the other polymers particularly at the molecular level. 

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