Single-Particle Mass Spectrometry of Titanium and Niobium Carbonitride Precipitates in Steels

Hegetschweiler, Andreas; Borovinskaya, Olga; Staudt, Thorsten; Kraus, Tobias

doi:10.1021/acs.analchem.8b04012

Cited by 27 publications

(19 citation statements)

References 42 publications

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“…This means that more than one quarter of the added niobium had already precipitated, prior precipitated on TiN or TiCN, and as a consequence lost for later strain-induced precipitation or precipitation strengthening. This was also found by Hegetschweiler et al [14], who used particle extraction methods. On the contrary, in niobium microalloyed steels without titanium, all niobium can be brought back into solution, as was shown by an APT study by Palmiere et al [32].…”

Section: Precipitation Behavior Before Tmcp Treatmentsupporting

confidence: 78%

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Tracing Microalloy Precipitation in Nb-Ti HSLA Steel during Austenite Conditioning

Webel

Herges

Britz

et al. 2020

Metals

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The microalloying with niobium (Nb) and titanium (Ti) is standardly applied in low carbon steel high-strength low-alloy (HSLA) steels and enables austenite conditioning during thermo-mechanical controlled processing (TMCP), which results in pronounced grain refinement in the finished steel. In that respect, it is important to better understand the precipitation kinetics as well as the precipitation sequence in a typical Nb-Ti-microalloyed steel. Various characterization methods were utilized in this study for tracing microalloy precipitation after simulating different austenite TMCP conditions in a Gleeble thermo-mechanical simulator. Atom probe tomography (APT), scanning transmission electron microscopy in a focused ion beam equipped scanning electron microscope (STEM-on-FIB), and electrical resistivity measurements provided complementary information on the precipitation status and were correlated with each other. It was demonstrated that accurate electrical resistivity measurements of the bulk steel could monitor the general consumption of solute microalloys (Nb) during hot working and were further complemented by APT measurements of the steel matrix. Precipitates that had formed during cooling or isothermal holding could be distinguished from strain-induced precipitates by corroborating STEM measurements with APT results, because APT specifically allowed obtaining detailed information about the chemical composition of precipitates as well as the elemental distribution. The current paper highlights the complementarity of these methods and shows first results within the framework of a larger study on strain-induced precipitation.

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Section: Precipitation Behavior Before Tmcp Treatmentsupporting

confidence: 78%

“…% niobium can be trapped in this way [12,13]. The amount of solute niobium effective for retarding recrystallization is therefore reduced [5,7,14]. This can be overcome by increasing the amount of niobium added to the steel.…”

Section: Introductionmentioning

confidence: 99%

Tracing Microalloy Precipitation in Nb-Ti HSLA Steel during Austenite Conditioning

Webel

Herges

Britz

et al. 2020

Metals

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show abstract

“…This would mean, that more than 1/4 of the added niobium is already precipitated, either on prior precipitated TiN or TiCN, and lost for later strain-induced precipitation or precipitation strengthening. This was also found by Hegetschweiler et al [14], who used particle extraction methods. On the contrary, in niobium microalloyed steels without titanium, all niobium can be brought back into solution, as was shown by an APT study by Palmiere et al [32].…”

Section: Precipitation Behavior Before Tmcp Treatmentsupporting

confidence: 78%

“…It has been found that up to 0.02 wt% niobium can be trapped in this way [12,13]. The amount of solute niobium effective for retarding recrystallization is therefore reduced [5,7,14]. This can be overcome by increasing the amount of niobium added to the steel.…”

Section: Introductionmentioning

confidence: 99%

Tracing Microalloy Precipitation in Nb-Ti HSLA Steel During Austenite Conditioning

Webel¹,

Herges²,

Britz³

et al. 2020

Preprint

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Microalloying of low carbon steel with niobium (Nb) and titanium (Ti) is standardly applied in high-strength low-alloy (HSLA) steels enabling austenite conditioning during thermo-mechanical controlled processing (TMCP), which results in pronounced grain refinement in the finished steel. The metallurgical effects of microalloying elements are related solute drag and precipitate particle pinning, both acting on the austenite grain boundary thereby delaying or suppressing recrystallization of the deformed grain. In that respect it is important to better understand the precipitation kinetics as well as the precipitation sequence in a typical Nb-Ti-microalloyed steel. Various characterization methods have been utilized in this study for tracing microalloy precipitation after simulating different austenite TMCP conditions in a Gleeble apparatus. Atom probe tomography (APT), scanning transmission electron microscopy in a focused ion beam equipped scanning electron microscope (STEM-on-FIB) and electrical resistivity measurements provide complementary information on the precipitation status and are correlated with each other. It will be demonstrated that accurate electrical resistivity measurements can monitor the general consumption of solute microalloys (Nb) during hot working which was complemented by APT measurements of the steel matrix. On the other hand, STEM revealed that a large part of Nb-containing particles during hot working are co-precipitated with titanium during cooling from the austenitizing temperature. Precipitates that form during cooling or isothermal holding can be distinguished from strain-induced precipitates by corroborating STEM measurements with APT results. APT specifically allows obtaining detailed information about the chemical composition of precipitates as well as the distribution of elements inside the particle. Electrical resistivity measurement, on the contrary, provides macroscopic information on the progress of precipitation and can be calibrated by APT. The current paper highlights the complementarity of these methods and shows first results within the framework of a larger study on strain-induced precipitation.

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“…Typical acquisition times (33-46 µs; Gschwind et al, 2011;Borovinskaya et al, 2013;Hendriks et al, 2017) are on the same order as the nanoparticle detection events (500 µs) (Olesik and Gray, 2012). Recent studies have demonstrated its utility in characterizing a variety of nanomaterials ranging from simple core-shell ENPs (Naasz et al, 2018) and multi-element steel NPs (Hegetschweiler et al, 2018) to more complex atmospheric nanoparticulates (Erhardt et al, 2019). Given this capability, ascertaining the sources of NPs may be possible by monitoring the respective elemental or isotopic ratios on a particle-by-particle basis (Praetorius et al, 2017;Montaño et al, 2019).…”

Section: Introductionmentioning

confidence: 99%

Quantification and Characterization of Nanoparticulate Zinc in an Urban Watershed

Bevers

Montaño

Rybicki

et al. 2020

Front. Environ. Sci.

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The recent expansion in the use of nanomaterials in consumer and industrial applications has led to a growing concern over their behavior, fate, and impacts in environmental systems. However, engineered nanoparticles comprise only a small fraction of the total nanoparticle mass in aquatic systems. Human activities, particularly in urban watersheds, are increasing the population of incidental nanoparticles and are likely altering the cycling of more abundant natural nanoparticles. Accurate detection, quantification, characterization, and tracking of these different populations is important for assessing both the ecological risks of anthropogenic particles, and their impact on environmental health. The urban portion of the South Platte watershed in Denver, Colorado (United States) was sampled for zinc to identify and quantify different nanomaterial sources. Single particle ICP-QMS was employed, to provide single elemental (Zn) signals arising from particle detection events. Coupling spICP-QMS to sample pre-fractionation (sedimentation, filtration) provided some insights into Zn association with nanoparticulate, colloidal, and suspended sediment phases. Single particle ICP-TOFMS (spICP-TOFMS) provided quantification across a large atomic mass range, yielding an even more detailed characterization (elemental ratios) on a particleby-particle basis, providing some delineation of multiple sources of particles. Across the watershed, on average, 21% of zinc mass was present as zinc-only particles with a rather uniform mean size of 40.2 nm. Zinc that was detected with one or more other elements, primarily Al, Fe, and Si, is likely to be present as heteroagglomerates or within mineral colloids. Although spICP-TOFMS provides a substantial amount of information, it is still in its early stages as an analytical technique and currently lacks the requisite sensitivity to study the smallest of nanoparticles. As this technique continues to develop, it is anticipated that this methodology can be broadly applied to study sources, behavior and effects of a disparate variety of nanoparticles from both geogenic and anthropogenic origins.

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Single-Particle Mass Spectrometry of Titanium and Niobium Carbonitride Precipitates in Steels

Cited by 27 publications

References 42 publications

Tracing Microalloy Precipitation in Nb-Ti HSLA Steel during Austenite Conditioning

Tracing Microalloy Precipitation in Nb-Ti HSLA Steel during Austenite Conditioning

Tracing Microalloy Precipitation in Nb-Ti HSLA Steel During Austenite Conditioning

Quantification and Characterization of Nanoparticulate Zinc in an Urban Watershed

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