The first stages of thermal relaxation towards equilibrium in a Zr57Ti5Cu20
Al10Ni8 bulk metallic glass have been studied by differential scanning calo
rimetry, X-ray diffraction, transmission electron microscopy and high-resol
ution electron microscopy. These coupled experiments rule out for this glas
s the existence of a phase separation on the nanometric scale preceding the
onset of crystallization. The first step of crystallization is of the prim
ary type, that is it consists of the nucleation of nanocrystallites in the
amorphous matrix with which they coexist in metastable equilibrium. The ver
y high nucleation rate leads to a nanometric composite structure with a num
ber density of about 7 x 10 m(3) of 3-4 nm crystallites, occupying a volume
fraction of about 15%. These features, as well as the crystallization kine
tics observed during isochronal or isothermal heating, are discussed.