ABSTRACT
Measuring local chemistry of specific crystallographic features by atom probe tomography (APT) is facilitated by using transmission Kikuchi diffraction (TKD) to help position them sufficiently close to the apex of the needle-shaped specimen. However, possible structural damage associated to the energetic electrons used to perform TKD is rarely considered and is hence not well-understood. Here, in two case studies, we evidence damage in APT specimens from TKD mapping. First, we analyze a solid solution, metastable ß-Ti-12Mo alloy, in which the Mo is expected to be homogenously distributed. Following TKD, APT reveals a planar segregation of Mo among other elements. Second, specimens were prepared near Σ3 twin boundaries in a high manganese twinning-induced plasticity steel, and subsequently charged with deuterium gas. Beyond a similar planar segregation, voids containing a high concentration of deuterium, i.e., bubbles, are detected in the specimen on which TKD was performed. Both examples showcase damage from TKD mapping leading to artefacts in the distribution of solutes. We propose that the structural damage is created by surface species, including H and C, subjected to recoil from incoming energetic electrons during mapping, thereby getting implanted and causing cascades of structural damage in the sample.
ABSTRACT
The worldwide development of electric vehicles as well as large-scale or grid-scale energy storage to compensate for the intermittent nature of renewable energy generation has led to a surge of interest in battery technology. Understanding the factors controlling battery capacity and, critically, their degradation mechanisms to ensure long-term, sustainable and safe operation requires detailed knowledge of their microstructure and chemistry, and their evolution under operating conditions, on the nanoscale. Atom probe tomography (APT) provides compositional mapping of materials in three dimensions with sub-nanometre resolution, and is poised to play a key role in battery research. However, APT is underpinned by an intense electric field that can drive lithium migration, and many battery materials are reactive oxides, requiring careful handling and sample transfer. Here, we report on the analysis of both anode and cathode materials and show that electric-field driven migration can be suppressed by using shielding by embedding powder particles in a metallic matrix or by using a thin conducting surface layer. We demonstrate that for a typical cathode material, cryogenic specimen preparation and transport under ultra-high vacuum leads to major delithiation of the specimen during the analysis. In contrast, the transport of specimens through air enables the analysis of the material. Finally, we discuss the possible physical underpinnings and discuss ways forward to enable shielding from the electric field, which helps address the challenges inherent to the APT analysis of battery materials.
ABSTRACT
The low yield strength (~300 MPa) of twinning-induced plasticity (TWIP) steels greatly limits their structural applications in the industrial field. Conventional strengthening mechanisms usually cause an enhancement of yield strength but also a severe loss of ductility. In this research, gradient substructures were introduced in the Fe-22Mn-0.6C TWIP steels by different pre-torsional deformation in order to overcome the above limitations. The substructure evolution, mechanical properties, and their origins in gradient-substructured (GS) TWIP steels were measured and compared by electron backscattered diffraction (EBSD), monotonous and loading-unloading-reloading (LUR) tensile tests. It was found that a simple torsional treatment could prepare gradient twins and dislocations in coarse-grained TWIP steel samples depending on torsional strain. The uniaxial tensile tests indicated that a superior combination of high yield strength, high ultimate strength, and considerable ductility was simultaneously obtained in the GS samples. The high yield strength and high ultimate tensile strength were attributed to synergetic strengthening mechanisms, viz., dislocation strengthening, due to the accumulation of high density of dislocations, and very high back stress strengthening due to gradient substructure distribution, which was accommodated through pile-ups of extra geometrically necessary dislocations (GNDs) across the sample-scale. Additionally, high ductility originated from gradient substructure-induced back stress hardening. The present study is also beneficial to the design efforts of high strength and high ductility of other heterogeneous-structured TWIP alloy systems.
