Probing Rubber Cross-Linking Generation of Industrial Polymer Networks at Nanometer Scale

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• 作者：Brice Gabrielle ; Emmanuel Gomez ; Jean-Pierre Korb
• 刊名：Journal of Physical Chemistry B
• 出版年：2016
• 出版时间：June 23, 2016
• 年：2016
• 卷：120
• 期：24
• 页码：5581-5589
• 全文大小：457K
• 年卷期：0
• ISSN：1520-5207

文摘

We present improved analyses of rheometric torque measurements as well as ¹H double-quantum (DQ) nuclear magnetic resonance (NMR) buildup data on polymer networks of industrial compounds. This latter DQ NMR analysis allows finding the distribution of an orientation order parameter (D_res) resulting from the noncomplete averaging of proton dipole–dipole couplings within the cross-linked polymer chains. We investigate the influence of the formulation (filler and vulcanization systems) as well as the process (curing temperature) ending to the final polymer network. We show that DQ NMR follows the generation of the polymer network during the vulcanization process from a heterogeneous network to a very homogeneous one. The time variations of microscopic D_res and macroscopic rheometric torques present power-law behaviors above a threshold time scale with characteristic exponents of the percolation theory. We observe also a very good linear correlation between the kinetics of D_res and rheometric data routinely performed in industry. All these observations confirm the description of the polymer network generation as a critical phenomenon. On the basis of all these results, we believe that DQ NMR could become a valuable tool for investigating in situ the cross-linking of industrial polymer networks at the nanometer scale.