In this paper we present self-designed mould suction casting apparatus allowing preparation of bulk samples in a form of rods (1.5 mm in diameter and about 3 cm in length). Making use of the apparatus the following compositions of Fe80Nb6B14, Fe76.2Nb5.7B13.8Gd4.8, Fe69.9Nb5.2B12.2Gd13, Fe76.2Nb5.7B13.8Y4.8, Fe69.9Nb5.2B12.2Y13, Fe61.5Nb4.6B10.8Y23.1 alloys were prepared. Phase and microstructure identification were curried out by making use of X-ray diffraction measurements. The obtained results show that the constructed apparatus fulfill all conditions required for such technique. Gadolinium as an alloying addition causes full amorphization in the case of the Fe76.2Nb5.7B13.8Gd4.8 alloy. In the other cases the structure was found to be nanocrystalline which is discussed in the paper.