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Size and Concentration Determination of Colloidal Nanocrystals by Small-Angle X-Ray Scattering

preprint
submitted on 02.03.2018 and posted on 02.03.2018 by Jorick Maes, Nicolo Castro, Kim De Nolf, Willem Walravens, Benjamin Abécassis, Zeger Hens

The accurate determination of the dimensions of a nano-object is paramount to the de- velopment of nanoscience and technology. Here, we provide procedures for sizing quasi- spherical colloidal nanocrystals (NCs) by means of small-angle x-ray scattering (SAXS). Using PbS NCs as a model system, the protocols outline the extraction of the net NC SAXS pattern by background correction and address the calibration of scattered x-ray intensity to an absolute scale. Different data analysis methods are compared, and we show that they yield nearly identical estimates of the NC diameter in the case of a NC ensemble with a monodisperse and monomodal size distribution. Extending the analysis to PbSe, CdSe

and CdS NCs, we provide SAXS calibrated sizing curves, which relate the NC diameter and the NC band-gap energy as determined using absorbance spectroscopy. In compari- son with sizing curves calibrated by means of transmission electron microscopy (TEM), we systematically find that SAXS calibration assigns a larger diameter than TEM calibration to NCs with a given band gap. We attribute this difference to the difficulty of accurately sizing small objects in TEM images. To close, we demonstrate that NC concentrations can be directly extracted from SAXS patterns normalized to an absolute scale, and we show that SAXS-based concentrations agree with concentration estimates based on absorption spectroscopy.

Funding

Ghent University (GOA 01G01513)

History

Email Address of Submitting Author

benjamin.abecassis@ens-lyon.fr

Email Address(es) for Other Author(s)

Zeger.Hens@UGent.be Jorick.Maes@ugent.be

Institution

Laboratoire de Chimie, CNRS, Ecole Normale Supérieure de Lyon

Country

France

ORCID For Submitting Author

0000-0002-1629-9671

Declaration of Conflict of Interest

No conflict of interest

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