Confocal Raman Microscopy as a Probe of Material Deconstruction in Processed Low-Density Polyethylene Particles.

IF 2.2 3区 化学 Q2 INSTRUMENTS & INSTRUMENTATION Applied Spectroscopy Pub Date : 2025-03-13 DOI:10.1177/00037028251322142
Md Wahiduzzaman, Jeremy Lawrence, Ashley Moreno-Gongora, Jiahe Xu, Dominick J Casadonte, Gerardine G Botte, Carol Korzeniewski
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引用次数: 0

Abstract

Confocal Raman microscopy was applied to detect structural change within individual particles of low-density polyethylene (LDPE) following chemical and electrochemical processing steps that aimed to facilitate material decomposition. A high numerical aperture (NA) oil-immersion objective enabled depth-profiling through the near surface region (20 μm-40 μm) of irregularly shaped particles with an axial spatial resolution < 2 μm estimated from measurements of instrument detection efficiency profiles. Changes in vibrational bands sensitive to polyethylene crystallinity were evident following treatments and linked to the release of low molecular weight compounds present as additives and products of processing. Effects of processing were probed by monitoring the rise of Raman scattering intensity in vibrational modes associated with polyethylene chains in a zig-zag (trans) conformation near 1128 cm-1, 1294 cm-1, and 1418 cm-1, signaling chain clustering and development of organized, crystalline-like assemblies. Pristine LDPE particles displayed a uniform structure across the near surface region, while particles treated initially with chemical extractant and then further processed displayed increasingly enhanced crystallinity up to the maximum depth probed (40 μm). As a step toward measurements on ensembles of particles, least squares modeling was adapted to derive pure component spectra reflecting crystallinity change within spectral datasets. The work demonstrates high spatial resolution Raman depth-profiling for the characterization of processed polymers using a high NA immersion objective to overcome the limitations of air-objectives often used for confocal Raman microscopy.

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共焦拉曼显微镜用于检测低密度聚乙烯(LDPE)单个颗粒在经过化学和电化学加工步骤后的结构变化,这些步骤的目的是促进材料分解。利用高数值孔径(NA)油浸物镜,可以对形状不规则的颗粒的近表面区域(20 μm-40 μm)进行深度剖析,其轴向空间分辨率分别为-1、1294 cm-1 和 1418 cm-1,显示了链的聚类和有组织的结晶状集合体的发展。原始的低密度聚乙烯颗粒在近表面区域显示出均匀的结构,而最初用化学萃取剂处理、然后进一步加工的颗粒在最大探测深度(40 μm)内显示出日益增强的结晶度。作为对颗粒集合进行测量的一个步骤,采用最小二乘建模法得出了反映光谱数据集内结晶度变化的纯组分光谱。这项研究利用高 NA 浸入式物镜,克服了共焦拉曼显微镜常用空气物镜的局限性,展示了用于表征加工聚合物的高空间分辨率拉曼深度剖面图。
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来源期刊
Applied Spectroscopy
Applied Spectroscopy 工程技术-光谱学
CiteScore
6.60
自引率
5.70%
发文量
139
审稿时长
3.5 months
期刊介绍: Applied Spectroscopy is one of the world''s leading spectroscopy journals, publishing high-quality peer-reviewed articles, both fundamental and applied, covering all aspects of spectroscopy. Established in 1951, the journal is owned by the Society for Applied Spectroscopy and is published monthly. The journal is dedicated to fulfilling the mission of the Society to “…advance and disseminate knowledge and information concerning the art and science of spectroscopy and other allied sciences.”
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