Anguy Yannick, Haurat Margaux, Dumon Michel
UMR CNRS 5295 laboratoire I2M, Université de Bordeaux, Talence, F-33405, France.
UMR CNRS 5629, laboratoire LCPO, Université de Bordeaux, Pessac, F-33600, France.
Small. 2025 Feb;21(5):e2405730. doi: 10.1002/smll.202405730. Epub 2024 Dec 23.
This work addresses the structural quantification of multiphase materials, here nanostructured polymer solid precursors and their micro/nano sized foamed counterparts. It is based on a strategy of contrast/edge enhancement, locally adaptive to image data in digital images of materials. The method allows to binarize straightforwardly the structures (the phases) in TEM and SEM images after edge identification, edge choice, and image virtual reconstruction. A detailed insight is brought into one-step batch supercritical CO foaming of acrylic amorphous PMMA (polymethyl methacrylate) polymers, aided by the nanostructuration of block copolymers (BCP), here MAM (butyl acrylate center block methyl acrylate side blocks). The foaming conditions, i.e., pressure drop rate (PDR) and saturation temperature required for an actual one-step procedure are specified and clarified, whereas previous works, dealing with "one-step procedures", are probably incurring in a two-step procedure. The roles of the BCP content (and size) and saturation temperature are carefully analyzed and further clarified, more comprehensively than in previous literature. Thanks to the analysis of size distributions of foams and foam blend precursors (0.25, 0.5, 10 wt% MAM), bi modality of 10 wt% foams is for example revealed. A discussion of kinetics effects, i.e., evolutions of the effective sample temperature T(t), and the effective glass transition temperature T(t). provides a new insight of "pseudo" one-step VS "real" one-step batch foaming.
这项工作致力于多相材料的结构量化,这里指的是纳米结构的聚合物固体前驱体及其微米/纳米尺寸的泡沫对应物。它基于一种对比度/边缘增强策略,该策略局部自适应于材料数字图像中的图像数据。该方法允许在边缘识别、边缘选择和图像虚拟重建后,直接对透射电子显微镜(TEM)和扫描电子显微镜(SEM)图像中的结构(相)进行二值化处理。借助嵌段共聚物(BCP)的纳米结构化,即甲基丙烯酸丁酯中心嵌段-甲基丙烯酸甲酯侧嵌段(MAM),对丙烯酸无定形聚甲基丙烯酸甲酯(PMMA)聚合物的一步间歇超临界CO₂发泡进行了详细研究。明确了实际一步法所需的发泡条件,即压降速率(PDR)和饱和温度,而以往处理“一步法”的工作可能实际上是两步法。与以往文献相比,更全面地仔细分析并进一步阐明了BCP含量(和尺寸)以及饱和温度的作用。通过对泡沫和泡沫共混前驱体(0.25、0.5、10 wt% MAM)尺寸分布的分析,例如揭示了10 wt%泡沫具有双峰性。对动力学效应,即有效样品温度T(t)和有效玻璃化转变温度T(t)的演变进行了讨论,为“伪”一步法与“真”一步间歇发泡提供了新的见解。