Enabling quantitative analysis of complex polymer blends by infrared nanospectroscopy and isotopic deuteration

Prine, Nathaniel; Cao, Zhiqiang; Zhang, Song; Li, Tianyu; Do, Changwoo; Hong, Kunlun; Cardinal, Camille; Thornell, Travis L.; Morgan, Sarah E.; Gu, Xiaodan

doi:10.1039/d3nr00886j

Title: Enabling quantitative analysis of complex polymer blends by infrared nanospectroscopy and isotopic deuteration

Journal Article · 04 April 2023 · Nanoscale

DOI: https://doi.org/10.1039/d3nr00886j · OSTI ID:1987770

^[1]; Cao, Zhiqiang ^[2];

^[1]; Li, Tianyu ^[3];

^[4];

^[3]; Cardinal, Camille ^[1];

^[5];

^[1];

^[1]

Univ. of Southern Mississippi, Hattiesburg, MS (United States)
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Sciences (CNMS)
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Sciences (CNMS); Univ. of Tennessee, Knoxville, TN (United States)
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
US Army Engineer Research and Development Center, Vicksburg, MS (United States)

Atomic-force microscopy coupled with infrared spectroscopy (AFM-IR) deciphers surface morphology of thin-film polymer blends and composites by simultaneously mapping physical topography and chemical composition. However, acquiring quantitative phase and composition information from multi-component blends can be challenging using AFM-IR due to the possible overlapping infrared absorption bands between different species. Isotope labeling one of the blend components introduces a new type of bond (carbon-deuterium vibration) that can be targeted using AFM-IR and responds at wavelengths sufficiently shifted toward unoccupied regions (around 2200 cm^–1). In this project, AFM-IR was used to probe the surface morphology and chemical composition of three polymer blends containing deuterated polystyrene; each blend is expected to exhibit various degrees of miscibility. AFM-IR results successfully demonstrated that deuterium labeling prevents infrared spectral overlap and enables the visualization of blend phases that could not normally be distinguished by other scanning probe techniques. The nanoscale domain composition was resolved by fast infrared spectrum analysis. Overall, we presented isotope labeling as a robust approach for circumventing obstacles preventing the quantitative analysis of multiphase systems by AFM-IR.

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Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source (SNS); Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Sciences (CNMS)

Sponsoring Organization:: US Army Engineer Research and Development Center (ERDC); USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF)

Grant/Contract Number:: AC05-00OR22725; PE 0603734A; W912HZ-18-C-0022

OSTI ID:: 1987770

Journal Information:: Nanoscale, Vol. 15, Issue 16; ISSN 2040-3364

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

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