Single crystals of the ternary clathrate-I compound K 4.2 Na 3.8 Si 46 were grown by a unique ion-exchange process employing spark plasma sintering (SPS). Single crystal structure refinements of clathrate-I K 4.2 Na 3.8 Si 46 at 100 and 300 K indicate that the 6d... Single crystal clathrate-I K 4.2 Na 3.8 Si 46 was synthesized by spark plasma sintering by simultaneous electrochemical redox and ion-exchange reactions using a NaSi and KCl as the precursor mixture. This method allows for the synthesis of kinetically metastable compounds, which are difficult to access by traditional synthetic methods as well as allows for the selective synthesis of clathrate-I and-II compositions by changing the reaction temperatures.
American Chemical Society
8 Sep 2015
Volume: 119 Issue: 37 Pages: 21745-21745
The Journal of Physical Chemistry C