Detailed study of the nanocasting process by in situ X-ray scattering and diffraction

A1 Journal article (refereed)

Internal Authors/Editors

Publication Details

List of Authors: Motolani Sakeye, Sebastian Ziller, Heinz Amenitsch, Mika Lindén, Jan-Henrik Smått
Publisher: American Chemical Society
Publication year: 2016
Journal: Journal of Physical Chemistry C
Journal acronym: J. Phys. Chem. C
Volume number: 120
Issue number: 3
Start page: 1854
End page: 1862
eISSN: 1932-7455


The nanocasting method is a valuable tool for producing metal oxides with a well-defined nanostructure. However, the precise details on how the metal oxide is
developed inside the mesoporous silica template remain unclear. In this study, we clarify how nickel nitrate species are evolving to nickel oxide and how they are redistributed inside mesoporous SBA-15 particles as a function of heating temperature and surrounding gas atmosphere by a combination of in situ small-angle X-ray scattering, X-ray diffraction and thermogravimetric techniques as well as ex situ transmission electron microscopy and nitrogen physisorption measurements. The SBA-15 template was initially impregnated with
Ni(NO3)2·6H2O using the wet infiltration method. The results indicate an initial redistribution of the nickel nitrate salt located outside the pore system into the mesopores due to dissolution, while at temperatures of 110−150 °C (depending on which type of gas flow is used) the mobility of the salt is lost due to drying of the salt. Above 220 °C, the nickel nitrate decomposes, possibly via nickel hydroxynitrate, to NiO, forming nanoparticles inside the pore channels. The results shed light on the events occurring during the nanocasting process and can be used for further optimization of the fidelity of replication.

Last updated on 2019-20-11 at 04:03