Investigation of the degree of cross-linking of polyethylene and thermosets using absolute optical spectroscopy and Raman microscopy

Abstract. In the research work presented here, an integrating sphere demonstrator which is suitable for the non-destructive determination of the degree of cross-linking or curing and has the potential for use as an at-line device for in-process quality assurance was assembled and explored. The measurement system allows the analysis of absorption and scattering coefficients of materials independently by means of absolute optical spectroscopy. The two optical parameters showed a good correlation with the degree of cross-linking of cross-linked polyethylene (PE-X) and the degree of curing of different thermosets and adhesives, each of which was determined using different reference methods (wet chemical analysis, differential scanning calorimetry (DSC), and dielectric analysis (DEA)). The results show that different PE-X materials can be distinguished well by their absorption and scattering in the visual (VIS) and near-infrared (NIR) wavelength range, respectively, and conclusions on their degree of cross-linking are possible. Also, the curing of resins can be monitored based on the absorption. In addition, Raman spectroscopy was used to achieve a better understanding of the material changes during the cross-linking of the materials. It also showed a good suitability for monitoring the curing processes in thermosets. In summary, the new method can be used to determine the crucial parameters of these industrial important material types and fulfils the great demand for fast, non-destructive testing, which can be carried out during the process or on the finished product.