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Abstract For the first time, high‐percentage molybdosilicic acid fiber mats (20–80% H 4 SiMo 12 O 40 ) were prepared using the electrospinning technique. The fiber mats were characterized by IR, XRD, and DSC. The results indicated that poly(vinyl alcohol) was changed from a semicrystalline to an amorphous state with an increasing molybdosilicic acid content. The results from scanning electron microscopy (SEM) showed that the average diameter of the fibers was about 285–600 nm. The effects of the viscosity and conductivity of the H 4 SiMo 12 O 40 /poly(vinyl alcohol) solution on the morphologies of the fiber mats were investigated. The swelling properties of the fiber mats in water were also studied.© 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 1573–1578, 2003
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