Rubber-Filler Interactions in Polyisoprene Filled with In Situ Generated Silica: A Solid State NMR Study

Borsacchi, Silvia; Sudhakaran, U. P.; Calucci, Lucia; Martini, Francesca; Carignani, Elisa; Messori, Massimo; Geppi, Marco

doi:10.3390/polym10080822

Cited by 15 publications

(14 citation statements)

References 33 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…HE and SE were combined to reconstruct the FID, which was fitted using the three components described above. Both the expected silica yield and the sol-gel reaction time determines the amount of bound rubber, probably due to different dispersion level obtained inside the rubber matrix [80]. To highlight the direct interaction of the polymer matrix with the filler, combined analysis of 1 H MQ NMR and equilibrium swelling data have been adopted.…”

Section: Polymer Physicsmentioning

confidence: 99%

Time Domain NMR in Polymer Science: From the Laboratory to the Industry

2019

View full text Add to dashboard Cite

Highly controlled polymers and nanostructures are increasingly translated from the lab to the industry. Together with the industrialization of complex systems from renewable sources, a paradigm change in the processing of plastics and rubbers is underway, requiring a new generation of analytical tools. Here, we present the recent developments in time domain NMR (TD-NMR), starting with an introduction of the methods. Several examples illustrate the new take on traditional issues like the measurement of crosslink density in vulcanized rubber or the monitoring of crystallization kinetics, as well as the unique information that can be extracted from multiphase, nanophase and composite materials. Generally, TD-NMR is capable of determining structural parameters that are in agreement with other techniques and with the final macroscopic properties of industrial interest, as well as reveal details on the local homogeneity that are difficult to obtain otherwise. Considering its moderate technical and space requirements of performing, TD-NMR is a good candidate for assisting product and process development in several applications throughout the rubber, plastics, composites and adhesives industry.

show abstract

Section: Polymer Physicsmentioning

confidence: 99%

Time Domain NMR in Polymer Science: From the Laboratory to the Industry

2019

View full text Add to dashboard Cite

show abstract

“…The interfacial dynamics appear unaffected by the silica phase in aggregated NR composites as those prepared by conducting the sol-gel process before the cross-linking reaction [35]. A recent solid state NMR study of polyisoprene samples filled with in situ generated silica indicates the presence of loosely bound rubber only experiencing a larger degree of mobility than that of a tightly bound rubber [36].…”

Section: Sol-gel In Situ Generation Of Filler Particlesmentioning

confidence: 99%

Natural Rubber Nanocomposites: A Review

Bokobza¹

2018

Nanomaterials

117

View full text Add to dashboard Cite

This paper reviews studies carried out on natural rubber filled with nanofillers such as spherical silica particles (generated by the sol gel reaction), clays and carbon nanostructures. It is shown that the mechanical response of NR is influenced by several parameters including the processing conditions, the state of filler dispersion, the polymer-filler interactions and the filler morphological aspects. Even if the sol gel process conducted in vulcanized rubber yields almost ideal dispersions, rod-shaped particles such as clay, carbon fibers or carbon nanotubes are by far more efficient in terms of mechanical reinforcement on account of their anisotropic character and their ability to orientate in the direction of stretch. The efficiency of layered fillers such as clays or graphitic structures clearly depends on the way they are dispersed (exfoliated) in the rubber. Complete exfoliation still remains difficult to achieve which limits the tremendous nanoreinforcement expected from a single layer of clay or graphite. In all cases, the onset of crystallization is observed at a lower strain value than that of the unfilled matrix due to strain amplification effects.

show abstract

“…Therefore, a strong connection exists between molecular mobility and 1 H time domain signals, with more mobile systems showing a more slowly decaying signal. Information on polymer dynamics can thus be obtained by FID analysis [ 25 , 26 , 27 ]. Here, FID’s of PVB-H and PVB-D were analyzed at different temperatures to track the dynamics, mainly associated to the α-relaxation, across the glass transition.…”

Section: Introductionmentioning

confidence: 99%

Unravelling Main- and Side-Chain Motions in Polymers with NMR Spectroscopy and Relaxometry: The Case of Polyvinyl Butyral

et al. 2021

Self Cite

View full text Add to dashboard Cite

Polyvinyl butyral (PVB) is an amorphous polymer employed in many technological applications. In order to highlight the relationships between macroscopic properties and dynamics at a microscopic level, motions of the main-chain and of the propyl side-chains were investigated between Tg − 288 °C and Tg + 55 °C, with Tg indicating the glass transition temperature. To this aim, a combination of solid state Nuclear Magnetic Resonance (NMR) methods was applied to two purposely synthesized PVB isotopomers: one fully protonated and the other perdeuterated on the side-chains. 1H time domain NMR and 1H field cycling NMR relaxometry experiments, performed across and above Tg, revealed that the dynamics of the main-chain corresponds to the α-relaxation associated to the glass transition, which was previously characterized by dielectric spectroscopy. A faster secondary relaxation was observed for the first time and ascribed to side-chains. The geometry and rate of motions of the different groups in the side-chains were characterized below Tg by 2H NMR spectroscopy.

show abstract

Rubber-Filler Interactions in Polyisoprene Filled with In Situ Generated Silica: A Solid State NMR Study

Cited by 15 publications

References 33 publications

Time Domain NMR in Polymer Science: From the Laboratory to the Industry

Time Domain NMR in Polymer Science: From the Laboratory to the Industry

Natural Rubber Nanocomposites: A Review

Unravelling Main- and Side-Chain Motions in Polymers with NMR Spectroscopy and Relaxometry: The Case of Polyvinyl Butyral

Contact Info

Product

Resources

About