Excess vacancies in nearly perfect alummum single crystals after slow cooling were investigated by high-temperature X-ray Lang camera. A series of topographs was taken 10℃, 20℃ and 50℃ intervals during the cooling process in the temperature range between 310℃ and 100℃. A Iot of black dots formed by excess vacancies were observed at 100℃. However, most of excess vacancies were contained in the form of small vacancy cluster undetected by X-ray Lang camera. And the cluster nucleated at impurity atom.