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We report on the morphological aspects of thin films prepared from a blue–green light‐emitting conjugated polymer, (methyl‐substituted ladder‐type poly(p‐phenylene, mLPPP)), blended with a solid‐state electrolyte composed either by a crown ether, dicyclohexano‐18‐crown‐6 (DCH18C6), or a high‐molecular‐weight poly(ethylene oxide) (HMWPEO), and a Li salt, lithium trifluoromethanesulfonate (LiCF3SO3, Li triflate (LiTf)), as they have been successfully applied in light‐emitting electrochemical cells (LECs). The surface morphologies of the blend layers were investigated using atomic force microscopy (AFM) in tapping mode, and the ion distribution was probed using X‐ray analysis by means of energy‐dispersive X‐ray spectrometry (EDXS) in the scanning electron microscope (SEM). We show that the two different phase‐separation processes, the complexation tendencies of the ionic species as well as the ionic transport numbers, have tremendous influence on the performances of the corresponding LECs, revealing either rectifying or symmetric optoelectronic characteristics in forward and reverse bias directions. This opens up new possibilities for tuning the optoelectronic properties of ion‐supported organic electronic devices.

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We here present the results of the first materials science analyses obtained with the prototype of a serial block-face sectioning and imaging tool, 3Viewtrade mark of Gatan, Inc (Pleasanton, CA, U.S.A.). It is a specially designed ultramicrotome operating in situ within an environmental scanning electron microscope originally developed for life science research. The microtome removes thin slices from the sample and the environmental scanning electron microscope images each new block surface of the specimen (serial block-face scanning electron microscopy). The Schottky emitter (FEG) of the microscope delivers high spatial resolution and has the advantage of stable performance and high durability. The slice thickness can typically be selected between 50 and 100 nm. It is possible to cut hundreds of slices and simultaneously acquire images with Digital Micrographtrade mark Model 700 (Gatan, Inc.). This article outlines the set-up and describes the automated process. The preparation of specimens for in situ ultramicrotomy is explained and the parameters for good image quality are discussed. In addition, special operative and analytic features of the controlling software are presented. Three different technical materials and one botanical specimen were analyzed delivering first results of this method for materials science and for botany.