The invention discloses a process for preparing a kind of gallium nitride nanoline of high purity, which employs gallium oxide (Ga2O3) as raw material, alkaline air (NH3) as reacting gas, inert gas argon gas (Ar) as protective gas, silicon board as base carrier for product growing, absolute ethyl alcohol, acetone and deionized water as cleaning agent for the sicicon board, and employs no accelerating agent; the gallium nitride nanoline grows out under the temperature of 950 Deg C and on the silicon board through ammonification reaction; the preparing process is simplified by grinding, sifting the raw material, cleaning the silicon board and quartz material, controlling the air extraction, argon gas and alkaline air inputting by tubing high temperature furnace control device procedurally, which prevents the side product generating effectively and increases the product outcome, purity and quality and finally getting the gallium nitride nanoline of light yellow, solid and in linary shape; the product is characterized by the uniform shape, order arrangement, and stable optical, chemical and physical property; the invention is characterized by the short preparing process, high yield (reaching to 95%), high purity (reaching to 98.6%) and the high linary accuracy, with the diameter being 5-20 cm, the average length of the monoline 30-50 ª–m.