Perspectives in 1H, 14N and 81Br solid-state NMR studies of interfaces in materials textured by self-assembled amphiphiles

Alonso, Bruno; Mineva, Tzonka; Innocenzi, Plinio; Trimmel, Gregor; Stubenrauch, Kurt; Melnyk, Inna V.; Zub, Yuriy L.; Fayon, Franck; Florian, Pierre; Massiot, Dominique

doi:10.1016/j.crci.2009.10.002

Cited by 16 publications

(16 citation statements)

References 93 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The most common and straightforward NMR methods for characterizing such silicate and hybrid networks are one-dimensional high-resolution experiments. However, NMR approaches are becoming more sophisticated at picking out specific interactions; further details of NMR techniques suitable for studying organicinorganic interfaces in silica hybrids are given by Babonneau et al [83] and the use of two-dimensional proton-based sequences by Alonso et al [84]. Another aspect of the advance of NMR methods is the combination of experimental NMR data and first principles calculations to provide additional structural insight, which has been applied to a conventionally formed 45S5 glass by Pedone et al [85].…”

Section: (E) Recent Advances In Sol-gel Glass Foamsmentioning

confidence: 99%

Characterizing the hierarchical structures of bioactive sol–gel silicate glass and hybrid scaffolds for bone regeneration

Martin

Sheng

Hanna

et al. 2012

Phil. Trans. R. Soc. A.

122

106

View full text Add to dashboard Cite

Bone is the second most widely transplanted tissue after blood. Synthetic alternatives are needed that can reduce the need for transplants and regenerate bone by acting as active temporary templates for bone growth. Bioactive glasses are one of the most promising bone replacement/regeneration materials because they bond to existing bone, are degradable and stimulate new bone growth by the action of their dissolution products on cells. Sol-gel-derived bioactive glasses can be foamed to produce interconnected macropores suitable for tissue ingrowth, particularly cell migration and vascularization and cell penetration. The scaffolds fulfil many of the criteria of an ideal synthetic bone graft, but are not suitable for all bone defect sites because they are brittle. One strategy for improving toughness of the scaffolds without losing their other beneficial properties is to synthesize inorganic/organic hybrids. These hybrids have polymers introduced into the sol-gel process so that the organic and inorganic components interact at the molecular level, providing control over mechanical properties and degradation rates. However, a full understanding of how each feature or property of the glass and hybrid scaffolds affects cellular response is needed to optimize the materials and ensure long-term success and clinical products. This review focuses on the techniques that have been developed for characterizing the hierarchical structures of sol-gel glasses and hybrids, from atomicscale amorphous networks, through the covalent bonding between components in hybrids and nanoporosity, to quantifying open macroporous networks of the scaffolds. Methods for non-destructive in situ monitoring of degradation and bioactivity mechanisms of the materials are also included.

show abstract

Section: (E) Recent Advances In Sol-gel Glass Foamsmentioning

confidence: 99%

Characterizing the hierarchical structures of bioactive sol–gel silicate glass and hybrid scaffolds for bone regeneration

Martin

Sheng

Hanna

et al. 2012

Phil. Trans. R. Soc. A.

122

106

View full text Add to dashboard Cite

show abstract

“…ZSM-5 was also studied by Abraham et al. [219], while Alonso and co-workers have reported similar studies on other mesoporous systems [220][221][222].…”

mentioning

confidence: 99%

Direct detection of nitrogen-14 in solid-state NMR spectroscopy

O’Dell¹

2011

Progress in Nuclear Magnetic Resonance Spectroscopy

View full text Add to dashboard Cite

“…Assessment of chain mobility: 1 H MAS NMR The 1 H MAS NMR spectra of the same three hybrid films (25,45 and 75 wt% P123) are depicted in Figure 5. Speciation in this spectrum is less trivial than the 13 C spectrum, and contradictory interpretations were reported in the literature [16,17]. The narrow feature at 1 ppm was straightforwardly attributed to the PPO methyl protons, but some difficulties arise for the massif spanning 2-4 ppm including the unresolved contributions from the CH and CH 2 protons.…”

Section: 22mentioning

confidence: 53%

“…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

View full text Add to dashboard Cite

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.

show abstract

Perspectives in 1H, 14N and 81Br solid-state NMR studies of interfaces in materials textured by self-assembled amphiphiles

Cited by 16 publications

References 93 publications

Characterizing the hierarchical structures of bioactive sol–gel silicate glass and hybrid scaffolds for bone regeneration

Characterizing the hierarchical structures of bioactive sol–gel silicate glass and hybrid scaffolds for bone regeneration

Direct detection of nitrogen-14 in solid-state NMR spectroscopy

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

Contact Info

Product

Resources

About