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Al-based composites used for hydrogen production were prepared by high-energy ball milling. The effect of the preparation parameters on the hydrolysis property of Al-based composites was investigated using the control variate method. The results indicate that the effect of preparation parameters—rotational velocity, milling duration, ball-to-powder mass ratio, and mass ratio of balls—have a significant effect on the hydrolysis property of Al-based composites. The hydrogen production yield and rate of Al-based composites with different parameters reach the peak values and then decrease as each respective parameter increases. The kinetic energy of Al-based composites transferred from milling tools increases with increasing preparation parameters, which results in better hydrolysis properties. However, when the value exceeds the threshold of preparation parameters, the hydrolysis property is prone to decline due to the agglomeration on the bottom or wall of the grinding jar. Furthermore, the mathematical correlation between the kinetic energy transferred from milling tools to Al-based composites and the rotational velocity was also discussed.

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