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Fiber mats of organic–inorganic hybrids, poly(vinyl alcohol) (PVA)/silica composite thin fibers, in the diameter of 200–400 nm were prepared by electrospinning. The fiber mats were characterized by IR, XRD, DSC, and TGA. The results indicated that PVA was changed from semicrystalline to amorphous state because of the increase of silica content. SEM photograph showed that junctions and bundles of the fiber mats decreased or almost disappeared, and bead increased with increasing silica content. Swelling property of the fiber mats was determined.