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A Combinatorial Approach to Reliable Quantitative Analysis of Small Nano-Sized Precipitates: A Case Study with α′ Precipitates in Fe–20 at% Cr Alloy

Published online by Cambridge University Press:  02 December 2021

Sudip Kumar Sarkar Open the ORCID record for Sudip Kumar Sarkar [Opens in a new window] ,
Deodatta Shinde Open the ORCID record for Deodatta Shinde [Opens in a new window] ,
Debasis Sen  and
Aniruddha Biswas
Sudip Kumar Sarkar*
Affiliation:
Materials Science Division, Bhabha Atomic Research Centre, Mumbai 400085, India Homi Bhabha National Institute, Mumbai 400094, India
Deodatta Shinde
Affiliation:
Materials Science Division, Bhabha Atomic Research Centre, Mumbai 400085, India
Debasis Sen
Affiliation:
Solid State Physics Division, Bhabha Atomic Research Centre, Mumbai 400085, India Homi Bhabha National Institute, Mumbai 400094, India
Aniruddha Biswas
Affiliation:
Materials Science Division, Bhabha Atomic Research Centre, Mumbai 400085, India Homi Bhabha National Institute, Mumbai 400094, India
*
*Corresponding author: Sudip Kumar Sarkar, E-mails: s.sudip.iitg@gmail.com; sudips@barc.gov.in
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Abstract

The quantitative characterization of small nano-sized precipitates poses genuine challenges and is often deficient in accuracy due to the inherent limitations inevitably associated with the individual experimental techniques. A convenient solution is to utilize multiple complementary techniques. The present work demonstrates an effective way to reliably quantify nano-sized precipitates using a combination of complementary techniques of atom probe tomography (APT), small angle neutron scattering (SANS), and transmission electron microscopy (TEM). As a case study, the size (radius, r), number density (NP), volume fraction (ϕ), and chemical composition of Cr-rich α′ precipitates are determined in Fe–20 at% Cr alloy, thermally aged at 773 K for 1,000 h. This combinatorial approach utilizes the strength of each technique in such a way that the overall accuracy of quantitative precipitation analysis improves significantly. For example, the superior spatial resolution makes TEM the appropriate technique to estimate the size and size distribution of the precipitates, while APT provides the chemical composition. Similarly, SANS analysis incorporates both the size and the compositional information thus derived independently and provides statiscally averaged quantitative analysis overcoming the field-of-view limitations of both TEM and APT. This combinatorial approach improves the accuracy of quantification and provides the true representation of the microstructure.

Keywords

APTcombinatorial approachnano-sized precipitatequantitative analysisSANSTEM
Type
Applications in Alloys
Information
Microscopy and Microanalysis , Volume 28 , Issue 4 , August 2022 , pp. 1370 - 1384
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Copyright
Copyright © The Author(s), 2021. Published by Cambridge University Press on behalf of the Microscopy Society of America

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