Characterizing Cross-Linking Within Polymeric Biomaterials in the SEM by Secondary Electron Hyperspectral Imaging
Characterizing Cross-Linking Within Polymeric Biomaterials in the SEM by Secondary Electron Hyperspectral Imaging
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DOI：
10.1002/marc.201900484
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发表时间：
2019-12-20
影响因子：
4.6
通讯作者：
Rodenburg, Cornelia
中科院分区：
文献类型：
--
作者：
Farr, Nicholas;Pashneh-Tala, Samand;Rodenburg, Cornelia
基于二次电子 (SE) 光谱的新颖功能为聚合物生物材料提供了增强的交联表征工具集，可在多尺度水平捕获交联密度和变化。自 1947 年以来，人们一直在研究 SE 光谱在材料表征方面的潜力。事实证明，缺乏合适的仪器和信号处理是将 SE 光谱应用于生物材料的障碍，因此，捕获包含交联信息的 SE 光谱是一个新概念。迄今为止，交联程度是通过核磁共振 (NMR)、差示扫描量热法和拉曼光谱 (RS) 等分析技术推断的。 NMR提供了原子尺度和分子尺度上极其局部的信息，而RS信息量则在微观尺度上。间接研究交联的其他方法是体积机械平均方法，例如拉伸和压缩模量测试。然而，这些用于估计聚合物交联密度的已建立的平均方法是不完整的，因为它们无法提供所有相关长度尺度上生物材料形态内的空间分布信息。本文通过分析不同甲基丙烯酸化程度的聚癸二酸甘油酯-甲基丙烯酸酯 (PGS-M) 证明了 SE 光谱功能的有效性，为 PGS-M 形态提供了新的见解。
A novel capability built upon secondary electron (SE) spectroscopy provides an enhanced cross-linking characterization toolset for polymeric biomaterials, with cross-linking density and variation captured at a multiscale level. The potential of SE spectroscopy for material characterization has been investigated since 1947. The absence of suitable instrumentation and signal processing proved insurmountable barriers to applying SE spectroscopy to biomaterials, and consequently, capturing SE spectra containing cross-linking information is a new concept. To date, cross-linking extent is inferred from analytical techniques such as nuclear magnetic resonance (NMR), differential scanning calorimetry, and Raman spectroscopy (RS). NMR provides extremely localized information on the atomic scale and molecular scale, while RS information volume is on the microscale. Other methods for the indirect study of cross-linking are bulk mechanical averaging methods, such as tensile and compression modulus testing. However, these established averaging methods for the estimation of polymer cross-linking density are incomplete because they fail to provide information of spatial distributions within the biomaterial morphology across all relevant length scales. The efficacy of the SE spectroscopy capability is demonstrated in this paper by the analysis of poly(glycerol sebacate)-methacrylate (PGS-M) at different degrees of methacrylation delivering new insights into PGS-M morphology.