Abstract

Accurate phase fraction analysis is an essential element of the microstructural characterization of alloys and often serves as a basis to quantify effects such as heat treatment or mechanical deformation. Additive manufacturing (AM) of metals, due to the intrinsic nonequilibrium solidification and spatial variability, creates additional challenges for the proper quantification of phase fraction. Such challenges are exacerbated when the alloy itself is prone to deformation-induced phase transformation. Using commonly available in-house X-ray diffraction (XRD) and electron backscatter diffraction (EBSD) and less commonly used synchrotron-based high-energy X-ray diffraction, we characterized nitrogen-atomized 17-4 precipitation-hardening martensitic stainless steel, a class of AM alloy that has received broad attention within the AM research community. On the same build, our measurements recovered the entire range of reported values on the austenite phase fractions of as-built AM 17-4 in literature, from ≈100% martensite to ≈100% austenite. Aided by Calphad simulation, our experimental findings established that our as-built AM 17-4 is almost fully austenitic and that in-house XRD and EBSD measurements are subject to significant uncertainties created by the specimen’s surface finish. Hence, measurements made using these techniques must be understood in their correct context. Our results carry significant implications, not only to AM 17-4 but also to AM alloys that are susceptible to deformation-induced structure transformation and suggest that characterizations with less accessible but bulk sensitive techniques such as synchrotron-based high energy X-ray diffraction or neutron diffraction may be required for proper understanding of these materials.

Highlights

  • Additive manufacturing (AM) of metals represents a suite of emerging manufacturing technologies that allow fabrication of parts with complex shapes and geometries in a single manufacturing step [1]

  • For AM alloys where post-build treatment is often required to eliminate undesired microstructural features such as unwanted phases [23], elemental micro-segregations [10], and microstructural anisotropy [24], or to take advantage of the alloy design and enhance the alloy performance [25], an accurate understanding of the as-built phase landscape serves as the starting point for the design of such post-build treatments

  • With an additional two-step ion milling, electron backscatter diffraction (EBSD) under identical measurement conditions shows an austenite level at 40.5%

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Summary

Introduction

Additive manufacturing (AM) of metals represents a suite of emerging manufacturing technologies that allow fabrication of parts with complex shapes and geometries in a single manufacturing step [1]. Previous studies have clearly demonstrated that, for many types of AM alloys, even when the starting feedstock materials have the correct composition and phases, due to the rapid solidification ubiquitous to AM, the as-built part can have either unexpected phases [6,7,8,9] or unexpected elemental distribution that can lead to unforeseen solid-state transformation during post processing [10,11,12,13,14] Because of these reasons, we must understand the effect of nonequilibrium solidification on the phase landscape of AM parts in their as-built states, which, in turn, forms a basis of the numerical models that pursue optimization strategies for fabrication and post-processing, a crucial component for the advancement of AM technologies due to their vast parameter space

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