A Combined SAXS/SANS Study for the in Situ Characterization of Ligand Shells on Small Nanoparticles: The Case of ZnO

Schindler T, Schmiele M, Schmutzler T, Kassar T, Segets D, Peukert W, Radulescu A, Kriele A, Gilles R, Unruh T (2015)

Publication Language: English

Publication Status: Published

Publication Type: Journal article, Original article

Publication year: 2015

Journal

Langmuir American Chemical Society

Publisher: American Chemical Society

Book Volume: 31

Pages Range: 10130-10136

Journal Issue: 37

DOI: 10.1021/acs.langmuir.5b02198

Abstract

ZnO nanoparticles (NPs) have great potential for their use in, e.g., thin film solar cells due to their electro-optical properties adjustable on the nanoscale. Therefore, the production of well-defined NPs is of major interest. For a targeted production process, the knowledge of the stabilization layer of the NPs during and after their formation is of particular importance. For the study of the stabilizer layer of ZnO NPs prepared in a wet chemical synthesis from zinc acetate, only ex situ studies have been performed so far. An acetate layer bound to the surface of the dried NPs was found; however, an in situ study which addresses the stabilizing layer surrounding the NPs in a native dispersion was missing. By the combination of small angle scattering with neutrons and X-rays (SANS and SAXS) for the same sample, we are now able to observe the acetate shell in situ for the first time. In addition, the changes of this shell could be followed during the ripening process for different temperatures. With increasing size of the ZnO core (dcore) the surrounding shell (dshell) becomes larger, and the acetate concentration within the shell is reduced. For all samples, the shell thickness was found to be larger than the maximum extension of an acetate molecule with acetate concentrations within the shell below 50 vol %. Thus, there is not a monolayer of acetate molecules that covers the NPs but rather a swollen shell of acetate ions. This shell is assumed to hinder the growth of the NPs to larger macrostructures. In addition, we found that the partition coefficient μ between acetate in the shell surrounding the NPs and the total amount of acetate in the solution is about 10% which is in good agreement with ex situ data determined by thermogravimetric analysis.

Authors with CRIS profile

Torben Schindler Professur für Nanomaterialcharakterisierung (Streumethoden) Martin Schmiele Professur für Nanomaterialcharakterisierung (Streumethoden) Tilo Schmutzler Professur für Nanomaterialcharakterisierung (Streumethoden) Thaer Kassar Professur für Nanomaterialcharakterisierung (Streumethoden) Doris Segets Lehrstuhl für Partikelsynthese (LFG) Wolfgang Peukert Lehrstuhl für Partikelsynthese (LFG) Tobias Unruh Professur für Nanomaterialcharakterisierung (Streumethoden)

Additional Organisation(s)

Graduiertenkolleg 1896/2 In situ Mikroskopie mit Elektronen, Röntgenstrahlen und Rastersonden Exzellenz-Cluster Engineering of Advanced Materials (EAM) Interdisziplinäres Zentrum, Center for Nanoanalysis and Electron Microscopy (CENEM)

Involved external institutions

Helmholtz-Zentrum Geesthacht Zentrum für Material- und Küstenforschung GmbH (HZG) DE Germany (DE) Forschungszentrum Jülich / Research Centre Jülich (FZJ) DE Germany (DE)

How to cite

APA:

Schindler, T., Schmiele, M., Schmutzler, T., Kassar, T., Segets, D., Peukert, W.,... Unruh, T. (2015). A Combined SAXS/SANS Study for the in Situ Characterization of Ligand Shells on Small Nanoparticles: The Case of ZnO. Langmuir, 31(37), 10130-10136. https://doi.org/10.1021/acs.langmuir.5b02198

MLA:

Schindler, Torben, et al. "A Combined SAXS/SANS Study for the in Situ Characterization of Ligand Shells on Small Nanoparticles: The Case of ZnO." Langmuir 31.37 (2015): 10130-10136.

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