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

Bhattacharya, Arunodaya; Parish, Chad M.; Henry, Jean; Katoh, Yutai

doi:10.1016/j.ultramic.2019.03.015

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

Journal Article · Thu Mar 28 00:00:00 EDT 2019 · Ultramicroscopy

DOI:https://doi.org/10.1016/j.ultramic.2019.03.015· OSTI ID:1505331

Bhattacharya, Arunodaya ^[1]; Parish, Chad M. ^[1]; Henry, Jean ^[2]; ^[1]

Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Univ. Paris-Saclay, Gif-sur-Yvette (France)

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. Furthermore 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.

View Accepted Manuscript (DOE)

Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Fusion Energy Sciences (FES); USDOE Office of Science (SC), Fusion Energy Sciences (FES) (SC-24)

Grant/Contract Number:: AC05-00OR22725

OSTI ID:: 1505331

Alternate ID(s):: OSTI ID: 1636489
OSTI ID: 23137821

Journal Information:: Ultramicroscopy, Journal Name: Ultramicroscopy Journal Issue: C Vol. 202; ISSN 0304-3991

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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Transmission Kikuchi diffraction

Data for: High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy. Bhattacharya, Arunodaya https://doi.org/10.17632/wsyx4sm548 The current record is supplemented by this dataset	dataset	January 2019
Data for: High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy. Bhattacharya, Arunodaya https://doi.org/10.17632/wsyx4sm548.1 The current record is supplemented by this dataset	dataset	January 2019

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

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