Due to recent technological development, requirements, and advances in Hi-Tech systems, the demands for a high vacuum atmosphere and its long-term preservation are important challenges. Chemical getters are appropriate candidates for this goal. In this research, the effect of milling and adding yttrium on getter performance in a Zr-Co based compound was studied. In this research, powder composition with 75%wt Zr and 25%wt Co as a control sample and powder composition with 75%wt Zr, 22% wt Co and 3% wt Y were milled in a high energy planetary ball mill for different times. To activate the getters, they were subjected to heat treatment. According to the vacuum preserving time in different samples, the optimum condition for heat treatment was heating at 360 °C for 80 min. The results showed that the addition of yttrium to the Zr-Co based getter reduced the activation temperature of 70 °C. The vacuum preserving time was evaluated in the range of 0.001–0.1 mmHg. In no getter case, this time was 345 s, and for unmilled and milled Zr75Co25 were 2080 and 3140 s, respectively; and for Zr75Co22Y3 this time was 4955 s. These values highlight the importance of using getter in vacuum systems, emphasize the impact of milling to achieve fine microstructure, as well as the paramount effect of yttrium as a catalyst.