H. Hofmeister et al., ATOMIC-STRUCTURE OF AMORPHOUS NANOSIZED SILICON POWDERS UPON THERMAL-TREATMENT, Physical review. B, Condensed matter, 54(4), 1996, pp. 2856-2862
Amorphous silicon powders prepared by plasma-enhanced chemical vapor d
eposition, of 8-24-nm-sized particles agglomerated into larger aggrega
tes were annealed in a reducing atmosphere to study the phase transfor
mation behavior of these particles. High-resolution electron microscop
y revealed a very rough surface, with structural details of 1 to 2 nm,
of the as-prepared single powder particles. Upon 1 h annealing at tem
peratures between 300 and 600 degrees C circular contrast features, 1.
5-2.5 nm in size, are observed in the amorphous particles, hinting to
the formation of a medium-range order. A distinct onset of crystalliza
tion is achieved at 700 degrees C, with structures ranging from very s
mall crystalline ordered regions of 2.5-3.5 nm in size, to fast-grown
multiply twinned crystallites. Rapid progress of crystallization, main
ly caused by growth twinning, is observed upon annealing at 800 degree
s C. At 900 degrees C, almost completely crystalline particles are for
med. The particles having lattice characteristics of diamond cubic sil
icon frequently exhibit a faulted structure, because of multiple twinn
ing events. They are covered by an amorphous oxide shell of a 1.5 to 2
nm thickness, which is found to develop with the onset of crystalliza
tion. Size and surface roughness of the as-prepared powders are widely
preserved throughout all stages of heating, and practically no sinter
ing occurs up to 900 degrees C.