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Primary crystallization of Ni(P) particles in hypoeutectic Ni–P amorphous alloy obtained by electroless deposition has been investigated with ASAXS. The particle size distribution, the size dependence of the particle composition and the amorphous matrix composition were found simultaneously. The size distribution consists of a peak at particle radius of ∼1 nm and a tail spanning from ∼2 to 15 nm. The composition of the particles of the peak changes from ∼14 to ∼2 at.% P as their radius grows from 0.7 to about 3 nm. The particles in the tail of the size distribution (2–15 nm) have nearly constant P content in the range of 0–2 at.%. The matrix composition tends to the eutectic one at the end of the primary crystallization process.