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PreprintCC BYChemRxiv

Spatially-Resolved Viscoelastic Response with AFM-IR

11 affiliations
  1. 1Department of Materials Science and Engineering
  2. 2Stanford University
  3. 3Department of Electrical and Computer Engineering
  4. 4University of Maryland
  5. 5Bruker Nano Surfaces Division
  6. 6Department of Chemistry
  7. 7Department of Chemical Engineering
  8. 8Department of Mechanical Engineering
  9. 9Kyushu University
  10. 10Nanoscale Device Characterization Division
  11. 11National Institute of Standards and Technology

Abstract

The viscoelastic response of phase-separated polymers systems may deviate from bulk values at the nanoscale. However, current measurement techniques lack the resolution to unmask local variations. We previously demonstrated the advantages of using a focused, pulsed infrared (IR) laser to photothermally heat a sample locally during nanomechanical measurements with an atomic force microscope (AFM), with heating controlled by varying the laser repetition rate. Herein, we demonstrate this IR heating coupled with nano-Dynamic Mechanical Analysis (nDMA). First, we measured the storage and loss modulus of a homogenous copolymer at varying IR repetition rates (i.e., at varying sample temperature), demonstrating a viscoelastic modulus response that is typical near the glass transition temperature. Further, we varied the IR laser repetition rate while modulating the AFM probe between 5 Hz and 100 Hz. With time-temperature superposition, modulus master curves were constructed through the Williams-Landel-Ferry relation, and the shift factors of IR heating-coupled nDMA curves were used to estimate the relation between IR repetition rate and surface temperatures. Lastly, this technique was applied to a phase-separated polymer blend to demonstrate the utility of the technique to decouple the viscoelastic behavior of different phases by leveraging the high spatial resolution of AFM.

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BibTeX
@misc{lim2026spatiallyresolved,
  title = {{Spatially-Resolved Viscoelastic Response with AFM-IR}},
  author = {Carina Yi Jing Lim and Jeffrey J. Schwartz and Bede Pittenger and Yuran Shi and Yoko Tomo and Peter De Wolf and Andrea Centrone and Zhenan Bao and Lukas Michalek},
  howpublished = {ChemRxiv},
  year = {2026},
  month = oct,
  doi = {10.26434/chemrxiv.15000735/v4},
  url = {https://chemrxiv.org/doi/full/10.26434/chemrxiv.15000735/v4},
  note = {CC BY},
}
RIS
TY  - UNPB
TI  - Spatially-Resolved Viscoelastic Response with AFM-IR
AU  - Carina Yi Jing Lim
AU  - Jeffrey J. Schwartz
AU  - Bede Pittenger
AU  - Yuran Shi
AU  - Yoko Tomo
AU  - Peter De Wolf
AU  - Andrea Centrone
AU  - Zhenan Bao
AU  - Lukas Michalek
PY  - 2026
DA  - 2026/10/02
PB  - ChemRxiv
DO  - 10.26434/chemrxiv.15000735/v4
UR  - https://chemrxiv.org/doi/full/10.26434/chemrxiv.15000735/v4
AB  - The viscoelastic response of phase-separated polymers systems may deviate from bulk values at the nanoscale. However, current measurement techniques lack the resolution to unmask local variations. We previously demonstrated the advantages of using a focused, pulsed infrared (IR) laser to photothermally heat a sample locally during nanomechanical measurements with an atomic force microscope (AFM), with heating controlled by varying the laser repetition rate. Herein, we demonstrate this IR heating coupled with nano-Dynamic Mechanical Analysis (nDMA). First, we measured the storage and loss modulus of a homogenous copolymer at varying IR repetition rates (i.e., at varying sample temperature), demonstrating a viscoelastic modulus response that is typical near the glass transition temperature. Further, we varied the IR laser repetition rate while modulating the AFM probe between 5 Hz and 100 Hz. With time-temperature superposition, modulus master curves were constructed through the Williams-Landel-Ferry relation, and the shift factors of IR heating-coupled nDMA curves were used to estimate the relation between IR repetition rate and surface temperatures. Lastly, this technique was applied to a phase-separated polymer blend to demonstrate the utility of the technique to decouple the viscoelastic behavior of different phases by leveraging the high spatial resolution of AFM.
ER  -