Fourier transform-infrared (FTIR) spectroscopy measurements were performed on a NEXUS (Thermo Nicolet) FTIR spectrometer employing an attenuated total reflectance (ATR) accessory model, Smart Performer. All spectra were obtained with a ZnSe crystal cell as the internal reflection element. Spectra were recorded in the 400 to 4,000 cm-1 wave number range by accumulating 64 scans at a resolution of 4 cm-1, subjected to data smoothing (15 points with the Savitzky-Golay method) and normalized to the 1,452 cm-1 peak before any data processing. Each spectrum was the average of at least three spectra measured in different areas of the sample. The crystallinity index was calculated as the intensity ratio between the two amide III components at 1260 cm-1 and 1230 cm-1 (C.I. = I1260/I1230) [28 (link)].
Differential scanning calorimetry (DSC) measurements were performed with a DSC Q200 instrument (TA Instruments, Waters, Milan, Italy). The scanned temperature ranged from room temperature to 400°C, at a heating rate of 10°C/minute. The analysis was carried out on samples of about 2 to 3 mg weight, in open aluminum pans of 40 μL volume, under N2 gas flux.