Abstract
Polymer nanocomposites are usually characterized using various methods, such as small angle X-ray diffraction (XRD) or transmission electron microscopy, to gain insights into the morphology of the material. The disadvantages of these common characterization methods are that they are expensive and time consuming in terms of sample preparation and testing. In this work, near infrared spectroscopy (NIR) spectroscopy is used to characterize nanocomposites produced using a unique twin-screw mini-mixer, which is able to replicate, at ~25 g scale, the same mixing quality as in larger scale twin screw extruders. We correlated the results of X-ray diffraction, transmission electron microscopy, G′ and G″ from rotational rheology, Young’s modulus, and tensile strength with those of NIR spectroscopy. Our work has demonstrated that NIR-technology is suitable for quantitative characterization of such properties. Furthermore, the results are very promising regarding the fact that the NIR probe can be installed in a nanocomposite-processing twin screw extruder to measure inline and in real time, and could be used to help optimize the compounding process for increased quality, consistency, and enhanced product properties.
Highlights
Layered silicates, such as nanoclays, are the most common nanofiller used in the polymer processing industry due to their potential of enhancing material properties and the fact that they are less expensive when compared to other nanofillers like carbon nanotubes or fullerene
The probe was connected to the spectrometer using fiber optics and the spectral data was collected with near infrared process spectrometer software (NIPS)
near infrared spectroscopy (NIR) measurements require reference investigations to achieve this link between mechanical properties and spectral data
Summary
Layered silicates, such as nanoclays, are the most common nanofiller used in the polymer processing industry due to their potential of enhancing material properties and the fact that they are less expensive when compared to other nanofillers like carbon nanotubes or fullerene. Various measurements are used for determining the formed structures (assessing intercalation vs exfoliation) and the homogeneity of the filler, including optical microscopy, scanning (SEM) and transmission (TEM) electron microscopy, mechanical (tensile strength, extensional rheology), and scattering methods (small angle (SAXS) and wide angle (WAXS) X-ray scattering). These are all time consuming, cost intensive, off-line methods and they do not have the possibility of being installed as an in-line measurement and quality control device directly in the production process. Following a more holistic approach, the scope of this paper is to apply NIR on a big number of off-line samples to ensure statistical stability with a large variety of properties and used characterization methods to show the possibilities and even more important the limits of this technology and gain information on possible one-for-all chemometric modeling strategies for quality control purposes
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