Vanadium–aluminum alloy is an important intermediate alloy for preparing aviation grade titanium alloys, and its product quality directly affects the finished product quality of titanium alloys. In this study, focusing on the problems of high powder content (19.8%) and low product yield in AlV55 alloy products, we conduct research on alloy quality control technology and implement a vanadium–aluminum alloy cooling crystallization control process. The research results indicate that there are three phases in AlV55 alloy, namely Al8V5, AlV, and Al2V3 phases. As the temperature decreases, the AlV phase gradually decomposes into Al8V5 phase and Al2V3 phase, and the proportion of Al8V5 phase is positively correlated with the fineness. Rapid cooling can reduce the formation of Al8V5 phase. The experimental results show that high-temperature water quenching can increase the proportion of vanadium–aluminum solid solution phase in the alloy from 19.03% to 31.76%, and reduce the fine powder rate to 13.2%, providing important product quality control means and technical support for the production of vanadium–aluminum alloys.