Synthesis of amorphous silicon colloids by trisilane thermolysis in high temperature supercritical solvents

Colloidal submicrometer-diameter amorphous silicon (a-Si) particles are synthesized with >90% yield by thermal decomposition of trisilane (Si3H8) in supercritical hexane at temperatures ranging from 400 to 500 degrees C and pressures up to 345 bar. A range of synthetic conditions was explored to optimize the quality of the product. Under the appropriate synthetic conditions, the colloids are spherical and unagglomerated. The colloids can be produced with average diameters ranging from 50 to 500 nm by manipulating the precursor concentration, temperature, and pressure. Relatively narrow particle size distributions, as measured by transmission electron microscopy (TEM), with standard deviations about the mean as low as approximately +/-10% could be obtained in some cases. We explored the thermal annealing of the amorphous silicon particles after isolation from the reactor and found that crystallization to diamond structure silicon occurred at temperatures as low as 650 degrees C. The amorphous and crystalline materials were characterized by X-ray diffraction and high resolution scanning and transmission electron microscopy.