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Plasma FIB Sample Preparation for In-Situ Synchrotron Studies of Additively Manufactured Alloys

Ga-free large-area sample preparation enables dynamic examination of precipitation expansion in Al-Mn-Cr-Zr alloys during material heat treatment

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Why Ga-Free Sample Preparation Is Essential for Synchrotron Studies of Precipitation Behavior

In-situ synchrotron experiments offer a powerful way to observe structural and chemical changes in real time, but to understand such a process the sample must retain its native chemistry. For aluminum alloys with complex precipitation behavior, gallium-based FIB preparation can affect grain boundary and devaluate the results of thermal analysis.

This workflow shows how large, representative samples can be precisely prepared using Xe⁺ plasma FIB. By avoiding Ga contamination, researchers successfully tracked Mn- and Cr-rich precipitates in an Al-Mn-Cr-Zr alloy under thermal load, capturing dynamic interactions critical to alloy design.

Why perform Ga-Free Sample Preparation

with TESCAN?

01
Root of the Problem

Why Traditional FIB Prep Fails for In-Situ Synchrotron Studies

Synchrotron imaging techniques like scanning X-ray fluorescence (s-XRF) require samples that are large enough to represent the overall material structure and precisely shaped for accurate measurements. Such precision can be achieved with FIB-SEM, while plasma FIB-SEM enables preparation of the larger sample dimensions required.

For precipitation studies in Al-Mn-Cr-Zr alloys, even minor gallium contamination can modify how precipitates behave near grain boundaries, producing misleading results during heat treatment.

Plasma FIB provides a cleaner alternative, enabling accurate, artifact-free tracking of microstructural evolution.

02
Materials and Methods

Large-Volume, Ga-Free Milling for Thermally Sensitive Alloys

The study focused on an Al-Mn-Cr-Zr alloy produced via powder bed fusion-laser beam (PBF-LB). A 10 mm³ bulk sample with >99.8% density was used. A site-specific lamella was extracted and thinned using the TESCAN AMBER X system with a Xe⁺ plasma ion beam, producing a sample approximately 10 µm tall, 30 µm wide, and 1 µm thick. It was mounted on a MEMS heating chip via Pt deposition.

The mounted sample was subjected to in-situ s-XRF imaging at the P06 beamline of the DESY synchrotron, where it underwent a simulated heat treatment with temperatures oscillating around 375 °C over a 24-hour period to monitor elemental movement.

03
Results and Discussion

Mn and Cr Precipitates Tracked with High Chemical Fidelity

s-XRF measurements revealed Mn-rich and Cr-rich precipitates forming along grain boundaries. Cr precipitates consistently formed near Mn phases, a behavior not observed in ex-situ studies. The as-printed melt pool microstructure remained unchanged, confirming thermal stability.

Crucially, the absence of Ga ensured that the grain boundary chemistry remained intact, allowing reliable interpretation of precipitate behavior. Plasma FIB also enabled larger lamella extraction with the exact dimensions required.

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Tescan Instruments & Technology

Used in This Workflow

TESCAN AMBER X 2

With high-current Xe⁺ ion milling and field-free SEM imaging, TESCAN AMBER X is engineered for sample preparation workflows that require chemical precision and large-volume trenching.

  • Ga-free Xe⁺ plasma FIB preserves sample chemistry – ideal for heat-sensitive alloys

  • Supports large, artifact-free lamella preparation for in-situ synchrotron workflows

  • Field-free UHR SEM imaging ensures topographical and compositional accuracy at microstructural boundaries
AMBER-X 2

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