Monitoring the evolution of polymer aging, especially early-stage aging, over both time and dimensionality can provide in-depth insight into aging-induced material invalidation and even disastrous accidents. However, it remains a great challenge because currently available methods for polymer aging only provide statistic results at a macroscopic scale. Herein, we report the first three-dimensional early-stage visualization (ESV) technique of polymer aging by using the fluorophore-bonded boronic acid to specifically target aging-induced hydroxyl groups through the B-O click reaction. This method can identify the initial aging of polypropylene (PP) as early as 20.0 min. In contrast, no signals can be detected by conventional infrared spectroscopy even after 21 days of thermal treatment. More importantly, the three-dimensional evolution for early-stage polymer aging was demonstrated: faster aggression in the horizontal plane (4.1 × 10-4 s-1) than in the vertical direction (2.6 × 10-9 m s-1) for PP films. The approach could undoubtedly provide valuable information in elucidating mechanistic details of polymer aging in three-dimensional scale and assessing the utility of advanced antiaging materials.
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