Cryogenic 4D-STEM analysis of an amorphous-crystalline polymer blend: Combined nanocrystalline and amorphous phase mapping.

Understanding and visualizing the heterogeneous structure of immiscible semicrystalline polymer systems is critical for optimizing their morphology and microstructure. We demonstrate a cryogenic 4D-STEM technique using a combination of amorphous radial profile mapping and correlative crystalline growth processing methods to map both the crystalline and amorphous phase distribution in an isotactic polypropylene (iPP)/ethylene-octene copolymer (EO) multilayer film with 5-nm step size. The resulting map shows a very sharp interface between the amorphous iPP and EO with no preferential crystalline structure near or at the interface, reinforcing the expected incompatibility and immiscibility of iPP and EO, which is a short-chain branched polyethylene.

Gallium, neon and helium focused ion beam milling of thin films demonstrated for polymeric materials: study of implantation artifacts.

Focused ion beam milling of ∼200 nm polymer thin films is investigated using a multibeam ion microscope equipped with a gallium liquid metal ion source and a helium/neon gas field-ionization source. The quality of gallium, neon, and helium ion milled edges in terms of ion implantation artifacts is analyzed using a combination of helium ion microscopy, transmission electron microscopy and light microscopy. Results for a synthetic polymer thin film, in the form of cryo-ultramicrotomed sections from a co-extruded polymer multilayer, and a biological polymer thin film, in the form of the base layer of a butterfly wing scale, are presented.