Strong changes in morphology and phase composition of zirconia nanoparticles can be induced by altering the growth conditions during nanoparticle synthesis. Here, we demonstrate that fractal ZrO 2 nanocrystals showing high specific surface area can be obtained in the nonaqueous synthesis by variation of temperature and precursor concentration. The growth process was studied in detail revealing a size increase from 2.7 to 7 nm as well as a change in the polymorphic composition from tetragonal to monoclinic zirconia. TEM measurements of samples withdrawn over the course of the synthesis showed that particles grow from roundish to dendritic shapes during the phase transformation. In contrast to the common assumption that the phase transition is controlled by thermodynamics, our data shows that the transition is rather governed by kinetics.
Microfluidic synthesis allows for a good control of the particle formation conditions while minimizing the consumption of material. In this study, we exploited these advantages for the nonaqueous synthesis of TiO 2 , ZnO and CeO 2 nanoparticles in a closed micro droplet reactor which resulted in well-defined particle structures. Monodisperse droplets are generated in microfluidic flow-focusing area and
The nonaqueous synthesis of zirconia nanoparticles was investigated and modeled by a comprehensive population balance equation framework that simulates the entire particle formation process to predict final nanoparticle properties as well as their evolvement during the synthesis.
This
study aims to elucidate the aggregation and agglomeration
behavior of TiO2 and ZrO2 nanoparticles during
the nonaqueous synthesis. We found that zirconia nanoparticles immediately
form spherical-like aggregates after nucleation with a homogeneous
size of 200 nm, which can be related to the metastable state of the
nuclei and the reduction of surface free energy. These aggregates
further agglomerate, following a diffusion-limited colloid agglomeration
mechanism that is additionally supported by the high fractal dimension
of the resulting agglomerates. In contrast, TiO2 nanoparticles
randomly orient and follow a reaction-limited colloid agglomeration
mechanism that leads to a dense network of particles throughout the
entire reaction volume. We performed in situ laser light transmission
measurements and showed that particle formation starts earlier than
previously reported. A complex population balance equation model was
developed that is able to simulate particle aggregation as well as agglomeration, which
eventually allowed us to distinguish between both phenomena. Hence,
we were able to investigate the respective agglomeration kinetics
with great agreement to our experimental data.
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