The present review analyses the recent literature on the combined use of X-ray microscopy (XRM) and atomic force microscopy (AFM) for multiscale characterization of Li+ (or Li) batteries (LiBs) with the aim of developing guidelines for correlative analysis. The usefulness of XRM resides in the capability of affording non invasively in situ images of the inner parts of a LiB (an encapsulated device) with spatial resolution of dozens of nm during operation. XRM is non destructive and affords the early diagnosis of LiBs degradation causes when these manifest themselves as microdeformations. Multiscale characterization of LiBs also requires AFM for visualizing the morphological/physical alterations of LiB components (anodes, cathodes, electrolyte) at the sub-nanometer level. Different to XRM, AFM necessitates of a modification of LiB working configuration since AFM uses a contacting probe whereas XRM exploits radiation-matter interactions and does not require LiB dissection. A description of the working principles of the two techniques is provided to evidence which technical aspects have to be considered for achieving a meaningful correlative analysis of LiBs. In delineating new perspectives for the analysis of LiBs we will consider additional complementary techniques. Among various AFM-based techniques particular emphasis is given to electrochemical AFM (EC-AFM).

The best strategy to tackle complexity when analyzing corrosion in iron artefacts is to combine different analytical methods. Traditional techniques provide effective means to identify the chemistry and mineralogy of corrosion products. Nevertheless, a further step is necessary to upgrade the understanding of the corrosion evolution in three dimensions. In this regard, Multiscale X-ray Microscopy (XRM) enables multi-length scale visualization of the whole object and provides the spatial distribution of corrosion phases. Herein, we propose an integrated workflow to explore corrosion mechanisms in an iron-nail from Motya (Italy) through destructive and non-destructive techniques, which permit the extraction of the maximum information with the minimum sampling. The results reveal the internal structure of the artefact and the structural discontinuities which lead the corrosion, highlighting the compositional differences between the tip and the head of the iron nail.

The diffusion of pollutants in the marine environment is nowadays a well-recognized issue that is attracting growing interest from the scientific and social communities. One of the possible strategies to study the effect of pollutants is to quantify their presence inside marine organisms that are directly exposed for a certain period to the polluted environment. Among them, mussels, commonly considered as “biological water filters”, stand out as ideal candidates since they are stationary animals and their food intake comes only from the filtering of the surrounding water. Thus, the evaluation of the accumulation of exogenous pollutants, in particular high-density or metallic, inside the mussel’s organs and specifically in its digestive glands, is of particular interest. In this paper we characterize the accumulation of exogenous materials in digestive glands of three different mussels by means of X-ray microscopy analysis. We provide evidence of how the unique capabilities of this technique allow reconstructing a full 3D image of an entire organ and how this image can provide valuable information to identify exogenous (non-biological) pollutants. Moreover, we take full advantage from the segmentation analysis of the images by discriminating different regions of the sample according to the density. With this experimental approach we measured the sizes of the exogenous pollutants and provided evidences that they accumulate preferentiality in the low-density regions of the organ, that are richer in ducts and secretive glands.

X-ray microscopy (XRM) is a non-destructive characterization technique that provides quantitative information regarding the morphology/composition of the specimen and allows to perform multiscale and multimodal 2D/3D experiments exploiting the radiation-matter interactions. XRM is particularly suitable to afford in situ images of inner parts of a battery and for the early diagnosis of its degradation in a non-invasive way. Since traditional characterization techniques (SEM, AFM, XRD) often require the removal of a component from the encapsu-lated device that may lead to non-desired contamination of the sample, the non-destructive multi-scale potential of XRM represents an important improvement to batteries investigation. In this work, we present the advanced technical features that characterize a sub-micron X-ray microscopy system, its use for the investigation of hidden and internal structures of different types of batteries and to understand their behavior and evolution after many charge/discharge cycles.

No abstract