Skutterudite Na1+xFe4P12 whiskers were prepared by a new hydrothermal reduc
tion alloying method. The diameter of the whisker is about 0.5-4 mum and it
s L/D ratio is about 10-20. Heating temperature and time can control the di
ameter and length of the skutterudite whisker. X-ray diffraction (XRD), sca
nning electron microscopy (SEM), transmission electron microscope (TEM), el
ectronic diffraction (ED), and X-ray fluorescence analysis have been employ
ed to characterize the products. XRD and ED revealed that the whiskers obta
ined at 200 degreesC are cubic skutterudite with a = 7.7995 Angstrom. X-ray
fluorescence analysis proved that there are sodium atoms in the skutterudi
te structure. The possible formation mechanism of Na1+xFe4P12 is proposed.