The paper introduced the preparation technology for bulk amorphous alloys. The samples were prepared by using the vacuum arc furnace, and the melt was processed by three different methods. The crystalloids of the samples were analyzed by using X - ray diffraction technology. The results showed that the compound oxide glass composed of B₂O₃ and Na₂SiO₃ reacted with some elements in the melt, therefore, it wasn´t favourable for coating the Zr₆₆Al₉Ni₉Cu₁₆ alloy, hence hindering the formation of the amorphous state. The fluorides composed of CaF₂(45%), A1F₃(50% ) and CaO (5%) and frace Ti0₂ reacted with some elements in the melt, so they were not suitable for purifying the Zr₆₆Al₉Ni₉Cu₁₆ alloy. High vacuum degree of equipment and high purity of the raw and processed materials were the important factors for to promoting the melt to form the amorphous alloy.