The invention relates to a non-aqueous electrolyte secondary battery, a negative electrode, a negative electrode material and a preparation of Si-O-Al composite. An Si-O-Al composite comprising silicon, silicon oxide, and aluminum oxide exhibits a powder XRD spectrum in which the intensity of a signal of silicon at 28.3 DEG is 1-9 times the intensity of a signal near 21 DEG. A negative electrode material comprising the Si-O-Al composite is used to construct a non-aqueous electrolyte secondary battery which is improved in 1st cycle charge/discharge efficiency and cycle performance while maintaining the high battery capacity and low volume expansion upon charging of silicon oxide.