The present invention provides a negative electrode material for a non-aqueous electrolyte secondary battery, comprising negative electrode active material particles containing a silicon compound expressed by SiOx at least partially coated with a carbon coating where 0.5≦̸x≦̸1.6. The negative electrode active material particles have a negative zeta potential and exhibiting fragments of CyHz compound in an outermost surface layer of the silicon compound when subjected to TOF-SIMS. This negative electrode material can increase the battery capacity and improve the cycle performance and battery initial efficiency. The invention also provides a negative electrode active material layer, a negative electrode, and a non-aqueous electrolyte secondary battery using this material, and a method of producing this material.