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

Abstract

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 M 23C 6, MX, M 7C 3, and M 2X ( 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 distinctmore » 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.« less

Authors:
 [1];  [1];  [2]; ORCiD logo [1]
  1. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
  2. Univ. Paris-Saclay, Gif-sur-Yvette (France)
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Fusion Energy Sciences (FES) (SC-24)
OSTI Identifier:
1505331
Grant/Contract Number:  
AC05-00OR22725
Resource Type:
Accepted Manuscript
Journal Name:
Ultramicroscopy
Additional Journal Information:
Journal Volume: 202; Journal Issue: C; Journal ID: ISSN 0304-3991
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; Nanoprecipitates; Transmission Kikuchi diffraction; HRTEM; Analytical electron microscopy; Multi-variate statistical analysis (MVSA)

Citation Formats

Bhattacharya, Arunodaya, Parish, Chad M., Henry, Jean, and Katoh, Yutai. High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy. United States: N. p., 2019. Web. doi:10.1016/j.ultramic.2019.03.015.
Bhattacharya, Arunodaya, Parish, Chad M., Henry, Jean, & Katoh, Yutai. High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy. United States. doi:10.1016/j.ultramic.2019.03.015.
Bhattacharya, Arunodaya, Parish, Chad M., Henry, Jean, and Katoh, Yutai. Thu . "High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy". United States. doi:10.1016/j.ultramic.2019.03.015.
@article{osti_1505331,
title = {High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy},
author = {Bhattacharya, Arunodaya and Parish, Chad M. and Henry, Jean and Katoh, Yutai},
abstractNote = {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.},
doi = {10.1016/j.ultramic.2019.03.015},
journal = {Ultramicroscopy},
number = C,
volume = 202,
place = {United States},
year = {2019},
month = {3}
}

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This content will become publicly available on March 28, 2020
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