High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy.

Statistically significant crystal structure and composition identification of nanocrystalline features such as nanoparticles/nanoprecipitates in materials chemistry and alloy designing using electron microscopy remains a grand challenge. In this paper, we reveal that differing crystallographic phases of nanoprecipitates in alloys can be mapped with unprecedented statistics using transmission Kikuchi diffraction (TKD), on typical carbon-based electron-transparent samples. Using a case of multiphase, multicomponent nanoprecipitates extracted from an improved version of 9% chromium Eurofer-97 reduced-activation ferritic-martensitic steel we show that TKD successfully identified more than thousand M23C6, MX, M7C3, and M2X (M=Fe, Cr, W, V, Ta; X = C, N) nanoprecipitates in a single scan, something that is currently unachievable using a transmission electron microscope (TEM) without incorporating a precision electron diffraction (PED) system. Precipitates as small as ∼20-25 nm were successfully phase identified by TKD. We verified the TKD phase identification using high-resolution transmission electron microscopy (HRTEM) and convergent beam electron diffraction (CBED) pattern analysis of a few precipitates that were identified by TKD on same sample. TKD study was combined with state-of-art analytical scanning transmission electron microscopy (STEM)-energy dispersive X-ray (EDX) spectroscopy and multivariate statistical analysis (MVSA) which provided the complete crystal structure and distinct chemistries of the precipitates in the steel in a high throughput automated way. This technique should be applicable to characterizing any multiphase crystalline nanoparticles or nanomaterials. The results highlight that combining phase identification by TKD with analytical STEM and modern data analytics may open new pathways in big data material characterization at nanoscale that may be highly beneficial for characterizing existing materials and in designing new materials.

Nitrogen adsorption data, FIB-SEM tomography and TEM micrographs of neutron-irradiated superfine grain graphite.

This manuscript provides raw nitrogen gas adsorption data, images and videos obtained from a technique that combines Focused Ion Beam (FIB) and Scanning Electron Microscopy (SEM) known as FIB-SEM tomography and Transmission Electron Microscopy (TEM) micrographs. This collection of data is useful for characterization of the effects of high fluence neutron irradiation in nuclear graphite as described in the associated manuscript, "Mesopores development in superfine grain graphite neutron-irradiated at high fluence" (Contescu et al., 2019). Nitrogen adsorption isotherms at 77 K are provided for graphite samples before and after neutron irradiation at 300, 450, and 750 °C at fluences before and after turnaround. FIB-SEM tomography reveals porosity of unirradiated and irradiated samples. Using this technique, four data sets were obtained, of which the first three are presented in video format, whereas the fourth one is a series of images provided in raw format unique to this manuscript. All microscopy data document the microstructure, surface area and porosity of superfine grain graphite G347A (Tokai Carbon, Japan) before irradiation and irradiated after turnaround at 400 °C. TEM micrographs provide unique information on irradiation damage at high neutron fluence (>27. 8 displacements per atom, dpa) in the microstructure and crystal lattice of graphite. Additional TEM micrographs are provided here, which do not duplicate the research paper published elsewhere (Contescu et al., 2019). These data sets are unique, as samples at high irradiation doses have never been measured or imaged before with the aforementioned techniques.

Irradiation-induced ß to α SiC transformation at low temperature.

We observed that ß-SiC, neutron irradiated to 9 dpa (displacements per atom) at ≈1440 °C, began transforming to α-SiC, with radiation-induced Frank dislocation loops serving as the apparent nucleation sites. 1440 °C is a far lower temperature than usual ß â†’ α phase transformations in SiC. SiC is considered for applications in advanced nuclear systems, as well as for electronic or spintronic applications requiring ion irradiation processing. ß-SiC, preferred for nuclear applications, is metastable and undergoes a phase transformation at high temperatures (typically 2000 °C and above). Nuclear reactor concepts are not expected to reach the very high temperatures for thermal transformation. However, our results indicate incipient ß â†’ α phase transformation, in the form of small (~5-10 nm) pockets of α-SiC forming in the ß matrix. In service transformation could degrade structural stability and fuel integrity for SiC-based materials operated in this regime. However, engineering this transformation deliberately using ion irradiation could enable new electronic applications.

Nanoscale engineering of radiation tolerant silicon carbide.

Radiation tolerance is determined by how effectively the microstructure can remove point defects produced by irradiation. Engineered nanocrystalline SiC with a high-density of stacking faults (SFs) has significantly enhanced recombination of interstitials and vacancies, leading to self-healing of irradiation-induced defects. While single crystal SiC readily undergoes an irradiation-induced crystalline to amorphous transformation at room temperature, the nano-engineered SiC with a high-density of SFs exhibits more than an order of magnitude increase in radiation resistance. Molecular dynamics simulations of collision cascades show that the nano-layered SFs lead to enhanced mobility of interstitial Si atoms. The remarkable radiation resistance in the nano-engineered SiC is attributed to the high-density of SFs within nano-sized grain structures that significantly enhance point defect annihilation.