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Precipitate number density determination in microalloyed steels by complementary atom probe tomography and matrix dissolution

  • Particle number densities are a crucial parameter in the microstructure engineering of microalloyed steels. We introduce a new method to determine nanoscale precipitate number densities of macroscopic samples that is based on the matrix dissolution technique (MDT) and combine it with atom probe tomography (APT). APT counts precipitates in microscopic samples of niobium and niobium-titanium microalloyed steels. The new method uses MDT combined with analytical ultracentrifugation (AUC) of extracted precipitates, inductively coupled plasma–optical emission spectrometry, and APT. We compare the precipitate number density ranges from APT of 137.81 to 193.56 × 1021 m−3 for the niobium steel and 104.90 to 129.62 × 1021 m−3 for the niobium-titanium steel to the values from MDT of 2.08 × 1021 m−3 and 2.48 × 1021 m−3. We find that systematic errors due to undesired particle loss during extraction and statistical uncertainties due to the small APT volumes explain the differences. The size ranges of precipitates that can be detected via APT and AUC are investigated by comparison of the obtained precipitate size distributions with transmission electron microscopy analyses of carbon extraction replicas. The methods provide overlapping resulting ranges. MDT probes very large numbers of small particles but is limited by errors due to particle etching, while APT can detect particles with diameters below 10 nm but is limited by small-number statistics. The combination of APT and MDT provides comprehensive data which allows for an improved understanding of the interrelation between thermo-mechanical controlled processing parameters, precipitate number densities, and resulting mechanical-technological material properties.

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Document Type:Article
Author:Louis V. WeberORCiD, Johannes WebelORCiD, Frank MücklichORCiD, Tobias KrausORCiD
Parent Title (English):Journal of materials science
First Page:12585
Last Page:12599
Date of Publication (online):2022/06/30
Year of first Publication:2022
Release Date:2022/08/03
Impact:04.682 (2021)
Funding Information:Aktien-Gesellschaft der Dillinger Hüttenwerke, Dillingen/Saar, Germany Companhia Brasileira de Metalurgia e Mineracao (CBMM) ZuMat Project funded by the European Regional Development Fund (ERDF) Deutsche Forschungsgemeinschaft (DFG, German Research Foundation) and the Federal State Government of Saarland (INST 256/298–1 FUGG).
DDC classes:600 Technik, Medizin, angewandte Wissenschaften / 660 Technische Chemie
Open Access:Open Access
Signature:INM 2022/062
Licence (German):License LogoCreative Commons - CC BY - Namensnennung 4.0 International