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Core–shell nanoparticles (CSNPs) have become indispensable in various industrial applications. However, their real internal structure usually deviates from an ideal core–shell structure. To control how the particles perform with regard to their specific applications, characterization techniques are required that can distinguish an ideal from a nonideal morphology. In this work, we investigated poly(tetrafluoroethylene)–poly(methyl methacrylate) (PTFE–PMMA) and poly(tetrafluoroethylene)–polystyrene (PTFE–PS) polymer CSNPs with a constant core diameter (45 nm) but varying shell thicknesses (4–50 nm). As confirmed by transmission scanning electron microscopy (T-SEM), the shell completely covers the core for the PTFE–PMMA nanoparticles, while the encapsulation of the core by the shell material is incomplete for the PTFE–PS nanoparticles. X-ray photoelectron spectroscopy (XPS) was applied to determine the shell thickness of the nanoparticles. The software SESSA v2.0 was used to analyze the intensities of the elastic peaks, and the QUASES software package was employed to evaluate the shape of the inelastic background in the XPS survey spectra. For the first time, nanoparticle shell thicknesses are presented, which are exclusively based on the analysis of the XPS inelastic background. Furthermore, principal component analysis (PCA)-assisted time-of-flight secondary-ion mass spectrometry (ToF-SIMS) of the PTFE–PS nanoparticle sample set revealed a systematic variation among the samples and, thus, confirmed the incomplete encapsulation of the core by the shell material. As opposed to that, no variation is observed in the PCA score plots of the PTFE–PMMA nanoparticle sample set. Consequently, the complete coverage of the core by the shell material is proved by ToF-SIMS with a certainty that cannot be achieved by XPS and T-SEM.
A scanning transmission X‐ray microscopy (STXM)‐based methodology is introduced for determining the dimensions (shell thickness, core and total diameter) of core‐shell nanoparticles, which exhibit a strong X‐ray absorption contrast and a well‐defined interface between core and shell material. A low radiation dosage during data acquisition and, therefore, less X‐ray beam‐induced damage of the sample is achieved by recording STXM images only at 2 predetermined energies of maximum Absorption contrast, instead of recording a stack of images across the whole absorption edge.
A model core‐shell nanoparticle, polytetrafluoroethylene (PTFE) cores with polystyrene (PS) shell, is used for demonstration. Near‐edge X‐ray absorption fine structure spectroscopy confirms the significant difference in X‐ray absorption behavior between PTFE and PS. Additionally, because of the insolubility of styrene in PTFE a well‐defined interface between particle core and shell is expected. To validate the STXM results, both the naked PTFE cores as well as the complete core‐shell nanoparticles are examined by scanning electron microscopy (SEM). The introduced STXM‐based methodology yields particle dimensions in agreement with the SEM results and provides additional information such as the position of the particle core, which cannot be extracted from a SEM micrograph.