Laboratory X-ray Microscopy Study of Microcrack Evolution in a Novel Sodium Iron Titanate-Based Cathode Material for Li-Ion Batteries

The long-term performance of batteries depends strongly on the 3D morphology of electrode materials. Morphological changes, i.e., particle fracture and surface deterioration, are among the most prominent sources of electrode degradation. A profound understanding of the fracture mechanics of electrode materials in micro- and nanoscale dimensions requires the use of advanced in situ and operando techniques. In this paper, we demonstrate the capabilities of laboratory X-ray microscopy and nano X-ray computed tomography (nano-XCT) for the non-destructive study of the electrode material’s 3D morphology and defects, such as microcracks, at sub-micron resolution. We investigate the morphology of Na0.9Fe0.45Ti1.55O4 sodium iron titanate (NFTO) cathode material in Li-ion batteries using laboratory-based in situ and operando X-ray microscopy. The impact of the morphology on the degradation of battery materials, particularly the size- and density-dependence of the fracture behavior of the particles, is revealed based on a semi-quantitative analysis of the formation and propagation of microcracks in particles. Finally, we discuss design concepts of the operando cells for the study of electrochemical processes.

A Study of Instantaneous Shear Mechanical Properties on the Discontinuity of Rock Mass Based on 3D Morphological Properties

In order to study the instantaneous mechanical properties of rock mass discontinuities with different 3D morphologies during the shear process, the Brazilian splitting method is used to prepare natural rock mass discontinuities, and the high-precision 3D scanning test of discontinuities is carried out. The Z 2 is selected as the evaluation parameter of the discontinuities. Based on the graded cyclic shear test results of discontinuities, the influence of the morphology characteristics on the strength and deformation characteristics is analyzed. With the increase of shear times, the 3D morphology characteristic parameters of the structural plane decrease steadily after the graded cyclic shear. Based on the test curve, the graded cyclic shear characteristics of rock mass discontinuities are analyzed from the shear deformation, and the shear process of the discontinuities is finely divided by combining with the variation characteristics of shear stiffness. Combined with the 3D morphology parameters, an empirical formula for the shear strength of discontinuities is proposed. Through verification, the effect of the new model is better than that of the classical JRC-JCS model.

3D Morphology Distribution Characteristics and Discrete Element Simulation of Sand-Gravel Mixtures

Sand-gravel mixtures are typical binary materials, exhibiting highly heterogeneous, discontinuous, and significant structural effects. The contact state between sand and gravel particles has a significant influence on the mechanical properties of the mixtures. This article focused on the complex internal structure and its mesostructural behavior of the mixtures, and a systematic statistical analysis was carried out to study the shape, size, and angularity of the coarse particles. The three-dimensional (3D) shapes of coarse aggregates were approximated to be hexahedron, pentahedron, and tetrahedron. An indicator called angularity and surface texture (AT) index was developed to characterize the combined effect of the coarse aggregate angularity and surface texture. Based on the screening testing and digital image processing, the particle size and AT index of aggregates were extracted, and their means, standard deviations, and statistical distributions were studied. An algorithm for generating 3D aggregates was developed based on the statistical results of the coarse aggregate 3D morphology. The coarse aggregate generating code was written using the fish language in PFC3D. The numerical model was then applied to conduct three typical monotonic or cyclic triaxial test simulations. Retrospective simulation of the laboratory tests using the proposed model showed good agreement, and the reliability of the model is effectively verified. The results interpreted well the mechanism of particle motion and the distribution of interparticle contact force during shearing from mesoscale of the mixtures, which can give better understanding and modeling of the nonlinear behavior of the sand-gravel mixtures.

Monitored Tomographic Reconstruction—An Advanced Tool to Study the 3D Morphology of Nanomaterials

Detailed and accurate three-dimensional (3D) information about the morphology of hierarchically structured materials is derived from multi-scale X-ray computed tomography (XCT) and subsequent 3D data reconstruction. High-resolution X-ray microscopy and nano-XCT are suitable techniques to nondestructively study nanomaterials, including porous or skeleton materials. However, laboratory nano-XCT studies are very time-consuming. To reduce the time-to-data by more than an order of magnitude, we propose taking advantage of a monitored tomographic reconstruction. The benefit of this new protocol for 3D imaging is that the data acquisition for each projection is interspersed by image reconstruction. We demonstrate this new approach for nano-XCT data of a novel transition-metal-based materials system: MoNi4 electrocatalysts anchored on MoO2 cuboids aligned on Ni foam (MoNi4/MoO2@Ni). Quantitative data that describe the 3D morphology of this hierarchically structured system with an advanced electrocatalytically active nanomaterial are needed to tailor performance and durability of the electrocatalyst system. We present the framework for monitored tomographic reconstruction, construct three stopping rules for various reconstruction quality metrics and provide their experimental evaluation.