Quantification of sulfur distribution on rubber surfaces by means of μ-X-ray fluorescence analysis

Abstract

A homogeneous distribution of sulfur in a rubber compound is often desired. Spatially resolved imaging techniques are useful for evaluating the distribution of this crosslinking chemical. Typical measurement methods such as SEM (scanning electron microscopy) or TEM (transmission electron microscopy) have very high resolutions. However, the sample size or the maximum area to be investigated is limited, which makes it difficult to obtain a statistically reliable determination of sulfur homogeneity across the component or sample.In this work, an alternative measurement technique is therefore presented: the μ-XRF (μ-X-ray fluorescence analysis). With the help of this method, it is possible to scan surfaces of several cm2 and to show the distribution of different chemical elements. Its measuring principle has been known for decades but has hardly been used in the rubber industry so far.The main reason for this is that its quantification process for polymeric samples is more complex than for geologic or metallic samples, which are typically been investigated with μ-XRF to date. In this paper, this issue is addressed and a solution is presented: With the help of the fundamental parameter method, the determination of sulfur homogeneity and distribution on rubber surfaces becomes possible. This opens up a variety of further possibilities for the use of μ-XRF in the rubber industry: For example, it could be used in areas of tire production, recycling of end-of-life rubber, and beyond.