Nuclear Magnetic Resonance as a Tool for the Investigation of Interfaces and Textures in Nanostructured Hybrid Materials

Alonso, Bruno; Bonhomme, Christian; Gervais, Christel; Guenneau, Flavien; Laurencin, Danielle; Ribot, François

doi:10.1002/9783527807130.ch20

Cited by 1 publication

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“…The objective of this work is to investigate the potential of solid-state nuclear magnetic resonance (NMR) analysis for the characterization of mesostructured polymer-silica hybrid films prepared by sol-gel chemistry with amphiphilic block copolymer template acting as template. Solid-state NMR spectroscopy has been already employed to characterize this class of materials, but mostly to determine the coordination status of silicon atoms [15], and in very few cases to examine the mesoscopic structure [16][17][18][19][20]. As sketched in Scheme 1, when a highly ordered mesoscopic order is achieved in polymer-silica hybrid (right image), the amphiphilic block copolymer is characterized by a spatial separation at the nanometer scale of the hydrophilic and hydrophobic segments.…”

Section: Introductionmentioning

confidence: 99%

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

et al. 2020

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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 1 H and 13 C magic angle spinning NMR spectra through the increase in chemical environment uniformity and chain mobility respectively, which both result from the self-assembly mechanism. 1 H NMR relaxation measurements (T 2 ) using low-field NMR spectroscopy are instrumental to identify the threshold template concentration where ordering takes place.

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