Formation Mechanism

Main content

Without detailed knowledge about how particles form in solution it is not possible to develop predictive synthesis approaches or to systematically improve existing synthesis methodologies. In the case of nonaqueous syntheses, where the particles are prepared in organic solvents, a complete reaction monitoring has to include the organic and the inorganic reactions as well as the organic-inorganic interface. Additionally, several orders of length and time scales have to be accessible, because the size of the species studied ranges from the molecular to the nano-, micro- and sometimes even macroscale, and the various chemical reactions might differ strongly in their rates. Such an exhaustive process observation is only possible by applying a variety of in-situ and ex-situ characterization tools. Finally, the experimental information has to be elaborated into a particle formation mechanism, thereby separating side reactions from those processes that are responsible for particle formation.

The mechanistic studies, especially all the in-situ experiments, are supervised by Dr. Dorota Koziej.

Our expertise in mechanistic studies can be summarized as follows:

  • Design of in-situ cells for synchrotron measurements
  • In-situ IR- and UV-vis reaction monitoring in a Mettler-Toledo batch reactor
  • In-situ X-ray absorption spectroscopy (XANES and EXAFS) and X-ray diffraction
  • Multivariate Curve Resolution−Alternating Least Squares (MCR-ALS) analysis
  • Organic reaction pathways in nonaqueous sol-gel syntheses
  • Study of classical and non-classical (i.e., particle-based) crystallization processes
  • Oriented attachment and mesocrystal formation

Selected references:

M. Staniuk, D. Zindel, W. van Beek, O. Hirsch, N. Kränzlin, M. Niederberger, D. Koziej, Matching the organic and inorganic counterparts during nucleation and growth of copper-based nanoparticles – in situ XANES, UV-Vis and IR spectroscopic studies, Cryst. Eng. Commun. 2015, in print

N. Kränzlin, W. van Beek, M. Niederberger, D. Koziej, Mechanistic Studies as a Tool for the Design of Copper-based Heterostructures, Adv. Mater. Interfaces 2015, 2, 1500094

N. Kränzlin, M. Staniuk, F. Heiligtag, L. Luo, H. Emerich, W. van Beek, M. Niederberger, D. Koziej, Rationale for the crystallization of titania polymorphs in solution, Nanoscale 2014, 6, 14716

O. Hirsch, G. Zeng, L. Luo, M. Staniuk, P. M. Abdala, W. van Beek, F. Rechberger, M. J. Süess, M. Niederberger, D. Koziej, Aliovalent Ni in MoO2 Lattice – Probing the Structure and Valence of Ni and its Implication on the Electrochemical Performance, Chem. Mater. 2014, 26, 4505

M. Staniuk, O. Hirsch, N. Kränzlin, R. Böhlen, W. van Beek, P. M. Abdala, D. Koziej, Puzzling Mechanism behind a Simple Synthesis of Cobalt and Cobalt Oxide Nanoparticles: In Situ Synchrotron X-ray Absorption and Diffraction Studies, Chem. Mater. 2014, 26, 2086

I. Olliges-Stadler, M. D. Rossell, M. Süess, B. Ludi, O. Bunk, J. S. Pedersen, H. Birkedal, M. Niederberger, Comprehensive Study of the Crystallization Mechanism Involved in the Nonaqueous Formation of Tungstite, Nanoscale 2013, 5, 8517

B. Ludi, M. J. Süess, I. A. Werner, M. Niederberger, Mechanistic Aspects of Molecular Formation and Crystallization of Zinc Oxide Nanoparticles in Benzyl Alcohol, Nanoscale 2012, 4, 1982


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