High-temperature and high-pressure pulsed synthesis apparatus for supercritical production of nanoparticles

In materials science continuous flow supercritical fluid reactors are widely used for highly controlled synthesis of nanoparticles. The major limitation of continuous flow reactors is that the inherent distribution of residence times leads to broadening of the corresponding size distribution of the nanoparticles, and in addition it is not possible to carry out synthesis with very short or very long reaction times. Here, we report a new synthesis concept that we call pulsed synthesis, which removes the limitations of flow synthesis at the expense of a more complex reactor design and extensive computer control. Another limitation of flow synthesis is that it is largely a black box, where limited direct information is available of the specific chemical reactions taking place, the particle nucleation, the particle growth, etc. Such information is commonly obtained from in situ synchrotron and neutron scattering studies, but transfer of information from in situ studies with static reactors to laboratory flow reactor conditions is highly non-trivial. The new pulse reactor provides superior heating rates, arbitrary residence times with narrow distribution limited only by the pulse duration, and the ability of using the same reactor both for nanoparticle production and in situ synchrotron studies; thus eliminating the need for transfer of in situ information to laboratory reactor designs. (C) 2011 American Institute of Physics. [doi:10.1063/1.3617419]