How precisely are solute clusters in RPV steels characterized by atom probe experiments?

TL;DR

This paper critically examines the precision of atom probe tomography in characterizing solute clusters in RPV steels, revealing measurement parameter influences and proposing a model-based approach to improve consistency and accuracy.

Contribution

It introduces a physical model to estimate true microstructures and demonstrates how measurement parameters affect reported cluster data, enhancing comparability across studies.

Findings

Measurement parameters significantly influence N and D values.

Model predictions align with experimental data when parameters are standardized.

Consistent analysis reduces data scatter and improves microstructure characterization.

Abstract

Atom probe tomography (APT) is a powerful microscopy technique to characterize nano-sized clusters of the alloying elements in the bulk of reactor pressure vessel (RPV) steels. These clusters are known to dominantly determine the evolution of mechanical properties under irradiation. The results are conventionally summarized as the overall number density N and the average diameter D of the solute clusters identified in the material. Here, we demonstrate that these descriptors are intrinsically imprecise because they are steered by the parameters involved in the measurement and data processing, some of which are directly under the control of the operators, but some others not. Consequently, a direct comparison between data derived at different laboratories is compromised, and key trends such as the evolution with dose, are masked. This study relies on a state-of-the-art physical model for neutron irradiation in steels to make reliable estimates of the true microstructure before the measurement is performed, which allows the prediction of the population of solute clusters that are not seen by APT. We mimic APT measurements from simulated microstructures, performing a detailed study of the effects of the parameters of the analysis. We show that the values of N and D reported in the scientific literature can be matched by the predictions of our theoretical model only if specific sets of parameters are used for each laboratory that issued the measurements. We also show that if, on the contrary, all studied cases are analyzed in a consistent way, the scatter of N and D values is reduced.