The catalytic performances of skeletal Cu prepared from Cu Ti amorphous alloy heated at various temperatures were tested for the hydrogen generation from ammonia borane. The catalytic activity per surface area decreased with increasing heating temperatures of Cu Ti amorphous alloy. The thermal treatment of Cu Ti amorphous alloy leads to the high surface area of skeletal Cu. A skeletal Cu catalyst prepared from heated Cu Ti amorphous alloy at 300°C which is a moderate temperature somewhat lower than crystallization temperature, exhibited a higher catalytic activity in this reaction.