Etching of LLDPE and LLDPE/HDPE blends

Despite its rapidly growing use in commercial applications, the morphology of LLDPE and its blends has not been thoroughly studied by microscopy techniques. As part of a study to examine the morphology of a LLDPE narrow fraction and its blends with HDPE via SEM, TEM and AFM, an appropriate etchant is required. However, no satisfactory recipes could be found in the literature. Mirabella used n-heptane, a solvent for LLDPE, as an etchant to reveal certain morphological features in the SEM, including faint banding in spherulites. A 1992 paper by Bassett included a TEM micrograph of an axialite of LLDPE, etched in a potassium permanganate solution, but no details were given. Attempts to use n-heptane, at 60°C, as an etchant were unsuccessful: depending upon thickness, samples swelled and increased in diameter by 5-10% or more within 15 minutes. Attempts to use the standard 3.5% potassium permanganate solution for HDPE were also unsuccessful: the LLDPE was severely overetched. Weaker solutions were also too severe.