An improved method for the matrix dissolution extraction of nanoparticles from microalloyed steel

Abstract

The chemical extraction of niobium and titanium carbonitride precipitates from microalloyed steels was studied. Steel samples and chemically synthesized reference nanoparticles were subjected to commonly used extraction protocols, and conditions were systematically varied. High acid concentrations led to particle etching with losses above 10%; long extraction times and small etchant volumes led to the formation of dense SiOx networks that engulfed the extracted particles. The addition of surfactants was found to reduce agglomeration and limit etching. We developed an optimized extraction protocol that can extract and retain particles with diameters below 10 nm with reduced etching and negligible network formation. The resulting particle dispersions are suitable both for efficient electron microscopy of large particle numbers in a single run and colloidal analysis of large numbers of particles in dispersion.

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Notes

  1. 1.

    The standard uses 5 g of steel that are dissolved in 100 mL HCl (6 mol L−1) and later filled up with 150 mL water.

  2. 2.

    V ∼ r3: a reduction of 15% in volume/mass goes along with a reduction of approx. 5% in radius.

  3. 3.

    For an image resolution with 2 pixels/nm and a particle size of 30 nm, the error in size determination is 1.6%.

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Acknowledgements

The authors would like to thank Eduard Arzt for his continuing support of the project. Andrea Jung is also acknowledged for the elementary analysis, Kathrin Alt for particle dissolution experiments, and Bastian Philippi for Matcalc Simulations.

Funding

This work was funded by the “AG der Dillinger Hüttenwerke” in Germany and a patent for a particle extraction procedure aided by a dispersant was submitted.

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Correspondence to Tobias Kraus.

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Hegetschweiler, A., Staudt, T. & Kraus, T. An improved method for the matrix dissolution extraction of nanoparticles from microalloyed steel. J Mater Sci 54, 5813–5824 (2019). https://doi.org/10.1007/s10853-018-03263-0

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