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A novel metrology strategy has been developed and applied to characterize the complex chemical transformations which are required to form spin-cast nanoporous low-K materials. Surface analysis based on Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) has been applied in static and dynamic modes, and coupled with X-ray Photoemission Spectroscopy (XPS), to observe the compositional and chemical bonding changes of the surface and the underlying thin film. Results show the cross-linking ofdoi:10.1063/1.1622526 fatcat:zqjo2s76zvexnlfmwxyg7ipyl4