Homogenous crystal nucleation and growth in polyamide 66 (PA66) are followed in situ by means of a combination of FTIR spectroscopy and fast scanning chip calorimetry (FSC). Therefore, a novel setup with a calorimetry chip equipped with an IR-transparent SiN membrane was developed, which enables to examine IR spectroscopic and FSC experiments on the identical specimen. Because of the small amount of sample material (~ 100 ng), it is possible to achieve heating and cooling rates up to 5000 Ks −1 , and hence to quench the sample into a fully amorphous state without quenched-in homogeneous crystal nuclei. Annealing the film then allows to determine the onset of homogenous nucleation and crystal growth by means of FSC, whereas molecular interactions are unraveled by FTIR spectroscopy. It is demonstrated that different moieties of PA66 respond distinctly during crystallization; far-reaching interactions such as hydrogen bonding are established prior to onset of short-range steric hindrance. Graphical Abstract Crystal nucleation and growth are followed in situ by means of a combination of FTIR spectroscopy and fast scanning chip calorimetry. For this purpose a novel IR-transparent chip enables to examine both measurements on the identical specimen, while heating and cooling rates up to 5000 Ks −1 and hence quenching into a fully amorphous state can be achieved

中文翻译：

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结合红外光谱和快速扫描芯片量热法研究聚酰胺 66 中均匀成核和晶体生长的指纹

通过 FTIR 光谱和快速扫描芯片量热法 (FSC) 的组合，在原位跟踪聚酰胺 66 (PA66) 中的均匀晶体成核和生长。因此，开发了一种配备有红外透明 SiN 膜的量热芯片的新型装置，可以在同一样品上检查红外光谱和 FSC 实验。由于少量的样品材料（~100 ng），可以实现高达 5000 Ks -1 的加热和冷却速率，从而将样品淬火成完全非晶态而没有淬火的均质晶核。然后对薄膜进行退火，可以通过 FSC 确定均匀成核和晶体生长的开始，而分子相互作用则通过 FTIR 光谱来解开。结果表明，PA66 的不同部分在结晶过程中反应明显；在短程位阻开始之前建立了深远的相互作用，例如氢键。图形摘要 通过 FTIR 光谱和快速扫描芯片量热法的组合，原位跟踪晶体成核和生长。为此，新型红外透明芯片能够检查同一样品的两种测量结果，同时加热和冷却速率高达 5000 Ks -1，因此可以实现淬火到完全非晶态 图形摘要 通过 FTIR 光谱和快速扫描芯片量热法的组合，原位跟踪晶体成核和生长。为此，新型红外透明芯片能够检查同一样品的两种测量结果，同时加热和冷却速率高达 5000 Ks -1，因此可以实现淬火到完全非晶态 图形摘要 通过 FTIR 光谱和快速扫描芯片量热法的组合，原位跟踪晶体成核和生长。为此，新型红外透明芯片能够检查同一样品的两种测量结果，同时加热和冷却速率高达 5000 Ks -1，因此可以实现淬火到完全非晶态