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The potential of electrospray deposition, for the controlled preparation of particles for imaging in electron microscopes, is evaluated on various materials: from mono-modal suspensions of spherical particles to multimodal suspensions and to real-world industrial materials. It is shown that agglomeration is reduced substantially on the sample carrier, compared with conventional sample preparation techniques. For the first time, it is possible to assess the number concentration of a tri-modal polystyrene suspension by electron microscopy, due to the high Deposition efficiency of the electrospray. We discovered that some suspension stabilizing surfactants form artifact particles during electrospraying. These can be avoided by optimizing the sprayed suspension.
Of many experimental techniques for measuring particle sizes and size distributions, electron microscopy (EM) is still considered as the gold standard, especially in the nano range (1–100 nm). Furthermore, high-resolution X-ray spectroscopy (EDX) in conjunction with EM can be applied to individul NPs.
Preparation of an EM sample for generic particulate materials is a difficult task. Usually, the particles in a suspension are deposited on a support. However, this procedure includes the drying of larger solvent amounts on the substrate itself, and this can affect the spatial distribution of the deposited particles. One possibility to overcome this is the use of an electrospray system, where the suspension of particles is sprayed onto the substrate in charged droplets that are so small that they either dry off on the substrate immediately without affecting the position of particles, or even already during their flight time to the substrate. Additionally, the charging of particles minimizes agglomeration and aggregation, maximizing the collection of the EM grids.
The prototype of an electrospray deposition System was tested. Electrospray is theoretically described since a long time, but no dedicated commercial instruments are available for the preparation of TEM grids yet, apart from electrostatic deposition of aerosols.
Several materials have been sprayed onto TEM grids and the resulting particle distributions were evaluated. Operation parameters such as the sample flow-rate, capillary – substrate distance, electric field strength and sampling period length have been optimized. It was found that the particles deposited by electrospray generally show a much more homogeneous spatial distribution on the substrate and a substantial increase of the number of single particles (suited to automatic analysis).
A combined methodical approach is tested with respect to the characterization of the inner structure of porous TiO2 layers as typically used in modern dye sensitized solar cells (DSSC). Their performance is directly linked to the surface area of the pore network. The micrometer thick layer employed was manufactured by screen-printing of a starting TiO2 powder constituted of shape-controlled, bipyramidal anatase nanoparticles on FTO/glass substrates. The analytical methods exploited in our study are Focused Ion Beam (FIB) slicing followed by 3D reconstruction as well as the new approach transmission Kikuchi diffraction (TKD) technology in the scanning electron microscope (SEM). Size and shape distribution of the TiO2 NPs within the layer can be extracted. SEM in transmission mode and atomic force microscopy (AFM) have been used to verify the dimensional data obtained by the new combined methodical approach. Its analytical benefits but also the challenges and limitations are highlighted.
Loss in efficiency of perovskite solar cells may be caused by structural and/or chemical alterations of the complex layered system. As these changes might take place either in the bulk and/or on the surface of the stratified material, analytical tools addressing both key issues are selected and combined. SEM/EDX combined with XPS were chosen as appropriate methodical approach to characterise perovskite laboratory cells in depth and complementary on top, before and after light exposure. The layered perovskite system investigated here is based on glass covered with fluorine doped tin oxide (FTO), followed by three porous thin films of TiO2, ZrO2 and a thick monolithic carbon. The TiO2 film is subdivided into a dense layer covered by a porous one constituted of nanoparticles with a truncated bipyramidal shape. This layered system serves as the matrix for the perovskite. After infiltration of perovskite solution and annealing, EDX
spectral maps on cross-sections of the specimen have been measured. The distribution of relevant
elements – Si, Sn, Ti, Zr and C – correlates conclusively with layers visible in the acquired SEM images. Lead and iodine are distributed throughout the porous layers C, ZrO2 and TiO2. In a SEM micrograph taken of the cross-section of a sample after illumination, the glass substrate and all layers FTO, TiO2, ZrO2 as well as C are clearly identified. By EDX it was found that several weeks of ambient daylight did not change significantly the qualitative elemental composition of lead and iodine throughout the solar cell system. It was confirmed with EDX that nanoparticles identified in high-resolution SEM micrographs contain mainly Pb and I, indicating these to be the perovskite
crystals. However, a time-dependent compositional and chemical altering was observed with XPS for the near-surface region of the outermost ~10 nm after two months of illumination.
The use of duplex stainless steels (DSS) in energy related applications is well known. Nowadays, DSS steels become more favorable than austenitic steels due to the outstanding mechanical properties, the good corrosion resistance and the lower nickel content. However, the use of the duplex grade in acidic environments such as seawater often leads to severe degradation of the structural integrity of the steel by hydrogen-induced/assisted cracking (HAC) phenomena, which can eventually result in premature failure. Hydrogen assisted degradation and cracking of steels are active fields of research even though this topic is intensively studied for more than a century. A bottleneck is the analytical validation of the theoretical models proposed ion the literature at the sub-micron scale.
Industrial and the research communities see a need for an accurate analytical method by which it is possible to image the distribution of hydrogen in the microstructure of a steels or and other alloys. Among the very few available methods hydrogen imaging methods, Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) has the principal capability for mapping of hydrogen in a steel’s microstructure. The combination of ToF-SIMS with multivariate data analysis (MVA), electron microscopy (SEM) and electron-backscattered diffraction (EBSD) is a powerful approach for providing chemical and structural information. The use of data fusion techniques has been shown recently to enhance the better understanding of the hydrogen induced degradation processes in in a DSS steel.
Several restoration projects of stained-glass windows have been performed in Poland since 2010.Chemical analysis of glass samples was performed with SEM/EDX on a FEI ESEM-XL 30, (EDX-EDAX) and with Micro-XRF (M4 Tornado, Bruker).The chemical composition of medieval glass samples and of glass samples of the 19th Century have been determined.
Scanning Electron Microscopy (SEM) or Transmission Electron Microscopy (TEM) ? This is a question, nowadays discussed in EM labs of research and industry involved in the characterization and metrology of nanoparticles. The Scanning principle is adapted to TEM, the Transmission mode is adapted to Ultra High Resolution SEM. Can modern SEM replace TEM, reach atomic resolution even without Cs corrector or nm lateral resolution for energydispersive X-ray spectroscopy (EDX)?
Due to the development of a New Cold Field Emission (NCFE) electron source Hitachi SEMs SU9000 and SU8200 can deliver routinely sub-nm image resolution and EDX mappings at very high count rates and a lateral EDX resolution of a few nm. A TiO2 sample provided by BAM was analysed at 30kV using low kV STEM – simultaneously with the Through-the-lens (TTL) SE detector, the Bright Field transmitted and Dark Field transmitted signals. By this method a pixel precise information of the particles surface using SE, its chemical nature using DF-STEM and its crystalline structure using Bright Field signal is given in one 40sec scan. The advantage of this observation mode compared to Ultra Low Voltage imaging is outlined.
The potential of electrospray deposition, for the controlled preparation of particles for imaging in electron microscopes, is evaluated on various materials: from mono-modal suspensions of spherical particles to multimodal suspensions and to real-world industrial materials. It is shown that agglomeration is reduced substantially on the sample carrier, compared with conventional sample preparation techniques. For the first time, it is possible to assess the number concentration of a tri-modal polystyrene suspension by electron microscopy, due to the high deposition efficiency of the electrospray. We discovered that some suspension stabilizing surfactants form artifact particles during electrospraying. These can be avoided by optimizing the sprayed suspension.