Chemical mapping of a block copolymer electrolyte by low-loss EFTEM spectrum-imaging and principal component analysis

Energy-filtered transmission electron microscopy spectrum-imaging (EFTEM SI) in the low electron energy-loss range is a valuable technique for probing the chemical structure of a material with nanoscale spatial resolution using a reduced electron dose. By analyzing EFTEM SI datasets using principal component analysis (PCA), the constituent chemical phases of the material can be identified in an efficient manner without prior knowledge of the specimen. We implement low-loss EFTEM SI together with PCA to investigate thin films of the block copolymer electrolyte poly(styrene-block-ethylene oxide) (PS-b-PEO) blended with a sodium salt. PCA identifies three main phases, the first and second phases corresponding to the two blocks of the copolymer and a third phase corresponding to the salt. The low-loss spectra for these phases are extracted from a noise-reduced EFTEM SI dataset and used to generate a chemical map of the material by multiple linear least square fitting. We validate the results of the low-loss EFTEM SI/PCA technique by applying the method to a control PS-b-PEO sample that does not contain the sodium salt, and by conducting spatially resolved X-ray energy-dispersive spectrometry on the salt-containing PS-b-PEO thin film.

Research highlights
► Chemical mapping of a block copolymer electrolyte is achieved.
► We investigate poly(styrene-block-ethylene oxide) blended with a sodium salt.
► Low-loss EFTEM spectrum-imaging and principal component analysis are performed.
► This is a convenient approach for radiation-sensitive materials.
► The sodium salt segregates to the interfacial regions of a lamellar block copolymer.