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Exploring complex transitions between polymorphs on a small scale by coupling AFM, FTIR and DSC: the case of Irganox 1076? antioxidant

机译:通过结合AFM,FTIR和DSC探索多晶型物之间的复杂过渡:Irganox 1076的情况?抗氧化剂

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This study illustrates the significant interest of using atomic force microscopy (AFM) in force curve imaging mode for discovering and studying not easily detectable solid/solid transitions between polymorphs: we show that AFM in this imaging mode is a powerful means for studying in situ these transitions as they can be (i) detected in a very early step because of the high spatial resolution (at nanometer scale) of AFM and (ii) be distinguished from melting/recrystallization processes that can occur in the same temperature range. This was illustrated with the case of Irganox 1076?. This compound is a phenolic antioxidant currently used in standard polymers; it can bloom on the surface of polymer-based medical devices and its polymorphism might affect the device surface state and thus the biocompatibility. In a previous paper, the polymorphism of this compound was studied: four forms were characterized at a macroscopic level and one of them (form III) was identified on the surface of a polyurethane catheter. However, it was difficult to characterize the transitions between the different forms with only classical tools (DSC, FTIR and SAXS). In the present study, to evidence these transitions, we use AFM measurements coupled with a heating stage and we correlate them to ATR-FTIR measurements and to DSC analysis. This new study put into evidence a solid–solid transition between form III and II.
机译:这项研究说明了在力曲线成像模式中使用原子力显微镜(AFM)来发现和研究多晶型之间不易检测到的固体/固体转变的巨大兴趣:我们证明,在这种成像模式下,AFM是研究的有力手段这些转变是可以原位发生的,因为(i)由于AFM具有很高的空间分辨率(纳米级),因此可以在很早的步骤中检测到这些转变,并且(ii)可以将其与熔化/重结晶过程区分开相同的温度范围。 Irganox 1076?的情况说明了这一点。该化合物是目前用于标准聚合物中的酚类抗氧化剂。它会在聚合物基医疗设备的表面上起霜,并且其多态性可能会影响设备的表面状态,从而影响其生物相容性。在先前的论文中,研究了该化合物的多态性:在宏观水平上表征了四种形式,并在聚氨酯导管表面上鉴定出其中一种形式(形式III)。但是,仅使用经典工具(DSC,FTIR和SAXS)很难描述不同形式之间的过渡。在本研究中,为证明这些转变,我们将AFM测量与加热阶段结合使用,并将它们与ATR-FTIR测量和DSC分析相关联。这项新的研究证明了形式III和形式II之间的牢固过渡。

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