Particle encapsulation techniques for atom probe tomography of precipitates in microalloyed steels

Webel, Johannes; Weber, Louis; Vardo, Emina; Britz, Dominik; Kraus, Tobias; Mücklich, Frank

doi:10.1016/j.ultramic.2021.113219

Cited by 5 publications

(2 citation statements)

References 41 publications

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“…According to Seol et al (2016), the surface modification from the conductive layer coating improves the overall evaporation sequences. Unlike ceramic coating approaches (Sundell et al, 2019;Webel et al, 2021), a high quality data could be acquired here because a fusible alloy has relatively high thermal (0.19 W/cm °C) and electrical conductivity (0.57 nΩ m) which allows to dissipate the energy and electrons quickly to the base of the specimen (Lipchitz et al, 2015). This can explain the high (3:3) success rate of sample preparation in this investigation, with over 10 million ions collected for each specimen, and without premature or microfractures.…”

Section: Summary and Discussionmentioning

confidence: 99%

A Liquid Metal Encapsulation for Analyzing Porous Nanomaterials by Atom Probe Tomography

Kim

El‐Zoka

Gault

2022

Microscopy and Microanalysis

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Analyzing porous (nano)materials via atom probe tomography has been notoriously difficult. Voids and pores act as concentrators of the electrostatic pressure, which results in premature specimen failure, and the electrostatic field distribution near voids leads to aberrations that are difficult to predict. In this study, we propose a new encapsulating method for porous samples using a low melting point Bi–In–Sn alloy, known as Field's metal. As a model material, we used porous iron made by direct-hydrogen reduction of single-crystalline wüstite. The complete encapsulation was performed using in situ heating on the stage of a scanning electron microscope. No visible corrosion nor dissolution of the sample occurred. Subsequently, specimens were shaped by focused ion-beam milling under cryogenic conditions at −190°C. The proposed approach is versatile and can be applied to provide good quality atom probe datasets from micro/nanoporous materials.

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Section: Summary and Discussionmentioning

confidence: 99%

A Liquid Metal Encapsulation for Analyzing Porous Nanomaterials by Atom Probe Tomography

Kim

El‐Zoka

Gault

2022

Microscopy and Microanalysis

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“…Apparent precipitate size and shapes can be affected by the so-called local magnification that is caused by different evaporation field strengths of adjacent phases [38]. The Nb precipitates cause a higher field strength than iron [54] and their shape will be somewhat distorted, but the large difference in precipitate morphology between both steels indicates that rather the particle nucleation and growth is the reason for the morphology differences [26]. The high solution temperature used for Steel Nb, quenching and successive aging at 690 °C caused Nb precipitation from a highly supersaturated ferrite matrix that has a low solubility for Nb.…”

Section: Minimum Detectable Precipitate Sizesmentioning

confidence: 99%

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

et al. 2022

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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. Graphical abstract

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Immobilization of essential oils in biopolymeric matrices: recent approaches for controlled delivery systems

Fernández-Quiroz,

Tohidi,

Paymard

et al. 2023

Studies in Natural Products Chemistry

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Particle encapsulation techniques for atom probe tomography of precipitates in microalloyed steels

Cited by 5 publications

References 41 publications

A Liquid Metal Encapsulation for Analyzing Porous Nanomaterials by Atom Probe Tomography

A Liquid Metal Encapsulation for Analyzing Porous Nanomaterials by Atom Probe Tomography

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

Immobilization of essential oils in biopolymeric matrices: recent approaches for controlled delivery systems

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