As was described above, as one of methods for increasing the battery capacity of the non-aqueous secondary battery, it has been studied to use the negative electrode that uses the silicon material as a main material as the negative electrode of the non-aqueous secondary batteries.

The non-aqueous electrolyte secondary battery that uses the silicon material is desired to have the cycle characteristics close to the same with the non-aqueous electrolyte secondary battery that uses a carbon material. However, a negative electrode material that shows the cycle safety equivalent with the non-aqueous electrolyte secondary battery that uses the carbon material has not been proposed. Further, since the silicon compound containing, in particular, oxygen has low initial efficiency compared with the carbon material, improvement of the battery capacity was limited by that amount.

There, by using a silicon oxide modified by insertion and partial desorption of Li as a negative electrode active material, a cycle retention rate and an initial efficiency of the battery have been improved.

However, due to modification with Li, the silicon oxide after modification has relatively low water resistance. Therefore, there was a problem such that stabilization of the silicon oxide after modification to slurry tends to be insufficient during preparation of the negative electrode.

There, the present inventors have conducted intensive studies about a production method of a negative electrode active material capable of obtaining excellent cycle characteristics and initial efficiency when used in the negative electrode of the non-aqueous electrolyte secondary batteries and came to complete the present invention.