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The surface and bulk chemistry of photoresist blends for use at the 157 nm node were analyzed using near edge x-ray absorption fine structure spectroscopy to quantify component segregation and identify surface phenomena that may impact pattern formation. Spectral combinations of the constituent polymers are used to fit the spectra of the blend films. Significant segregation of one component to the surface of the photoresist film was found, in excess of the composition of that component in the blend. The bulk data were consistent with initial blend compositions. As expected, the more hydrophobic or lower surface tension component wets the film surface even under typical photoresist processing conditions. © 2003 American Vacuum Society.