Assessing mesoscopic organization in copolymer-templated silica hybrid films via solid-state nuclear magnetic resonance

•Solid-state nuclear magnetic resonance (NMR) reveals ordering in hybrid silica film.•Narrower 1H NMR lines reflect a better chemical uniformity of ordered structures.•Narrower 13C NMR lines translate a higher mobility of ordered structures.•Disorder-to-order transition is reflected by 1H transverse relaxation time. In the context of increasing use of nanostructured materials, finding innovative characterization methods able to assess precisely the level of ordering is essential. To this end, a range of model organic-inorganic copolymer-silica films is synthesized using poly(ethylene oxide)-b-poly(propylene oxide)-b-poly(ethylene oxide) amphiphilic triblock copolymer as supramolecular template. Upon increasing copolymer concentration (10–100 wt%), the order can be gradually enhanced from short-range to long-range as proved by conventional techniques such as X-ray diffraction and electron microscopy. To evaluate the level of mesoscopic organization, the same series of samples is also analyzed by solid-state nuclear magnetic resonance (NMR) spectroscopy. The disorder-to-order transition is probed by 1H and 13C magic angle spinning NMR spectra through the increase in chemical environment uniformity and chain mobility respectively, which both result from the self-assembly mechanism. 1H NMR relaxation measurements (T2) using low-field NMR spectroscopy are instrumental to identify the threshold template concentration where ordering takes place.