TY - JOUR A1 - Guilherme, A. A1 - Hodoroaba, Vasile-Dan A1 - Benemann, Sigrid A1 - Coroado, J. A1 - Carvalho, M.L. T1 - Morphological and compositional features of blue and yellow pigments used in Portuguese glazed ceramics by SEM/EDX - unravelling manufacturing differences N2 - Morphological and compositional features regarding blue and yellow pigments used in glazed ceramics from Portugal are investigated by means of a SEM/EDX system. Fragments of samples produced in the main pottery-making centres between the XVI–XVIII centuries (Lisbon and Coimbra) were the objects of study. The main question to be answered is whether there are differences in the manufacturing procedures employed. For this purpose, two types of samples were analysed: faiences and wall-tiles (the famous 'Azulejos', in Portuguese). Differences between the manufacturing techniques of the two production centres were veritably found. The expected linkage between Fe–Co–Ni–As–Bi was challenging to investigate. Thus, Co was found in Fe- or Ni-rich structures, but with no structural connection to As or Bi. However, the As-needle-like structures were always identified in blue regions. One interesting finding related particularly to the blue pigment was the presence of SnO2 agglomerates throughout the whole glaze, which suggests its intentional addition for 'lightening' the well known dark Co blue. Concerning the yellow pigment differences established in the crystal shape and size are indicative of different firing temperatures used. KW - Scanning electron microscope (SEM) KW - Energy dispersive X-ray spectroscopy (EDX) KW - Portuguese glazed ceramics KW - Coimbra KW - Lisbon KW - Blue pigment KW - Yellow pigment KW - Morphology KW - Elemental composition KW - Firing temperature PY - 2014 DO - https://doi.org/10.1039/c3ja50268f SN - 0267-9477 SN - 1364-5544 VL - 29 IS - 1 SP - 51 EP - 57 PB - Royal Society of Chemistry CY - London AN - OPUS4-29722 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Benemann, Sigrid A1 - Motzkus, C. A1 - Macé, T. A1 - Palmas, P. A1 - Vaslin-Reimann, S. T1 - Advanced analysis of spherical SiO2 aerosol nanoparticles with a high-resolution SEM KW - Spherical nanoparticles KW - SiO2 KW - SEM KW - Transmission-SEM KW - VAMAS PY - 2012 DO - https://doi.org/10.1017/S1431927612010604 SN - 1431-9276 SN - 1435-8115 VL - 18 IS - Suppl. 2 SP - 1750 EP - 1751 PB - Cambridge University Press CY - New York, NY AN - OPUS4-26749 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Anja A1 - Heinrich, Thomas A1 - Tougaard, S. A1 - Werner, W. S. M. A1 - Hronek, M. A1 - Kunz, Valentin A1 - Radnik, Jörg A1 - Stockmann, Jörg M. A1 - Hodoroaba, Vasile-Dan A1 - Benemann, Sigrid A1 - Nirmalananthan-Budau, Nithiya A1 - Geißler, Daniel A1 - Sparnacci, K. A1 - Unger, Wolfgang T1 - Determining the thickness and completeness of the shell of polymer core-shell nanoparticles by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and transmission scanning electron microscopy N2 - 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. KW - XPS KW - T-SEM KW - ToF-SIMS KW - Core-shell nanoparticles PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-499165 DO - https://doi.org/10.1021/acs.jpcc.9b09258 VL - 123 IS - 49 SP - 29765 EP - 29775 PB - American Chemical Society CY - Washington, DC AN - OPUS4-49916 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -