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Title: Revealing nanoscale dynamics during an epoxy curing reaction with x-ray photon correlation spectroscopy

Abstract

In this work the evolution of nanoscale properties is measured during the thermally triggered curing of an industrial epoxy adhesive. We use x-ray photon correlation spectroscopy (XPCS) to track the progression of the curing reaction through the local dynamics of filler particles that reflect the formation of a thermoset network. Out-of-equilibrium dynamics are resolved through identification and analysis of the intensity– intensity autocorrelation functions obtained from XPCS. The characteristic time scale and local velocity of the filler is calculated as functions of time and temperature. We find that the dynamics speed up when approaching the curing temperature (Tcure), and decay rapidly once Tcure is reached. We compare the results from XPCS to conventional macroscale characterization by differential scanning calorimetry (DSC). The demonstration and implementation of nanoscale characterization of curing reactions by XPCS proves useful for future development and optimization of epoxy thermoset materials and other industrial adhesive systems.

Authors:
ORCiD logo [1];  [2];  [2];  [3];  [2];  [4]; ORCiD logo [5];  [6]; ORCiD logo [2]
  1. Stony Brook Univ., NY (United States); Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)
  2. Stony Brook Univ., NY (United States)
  3. Cornell Univ., Ithaca, NY (United States)
  4. Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)
  5. Adhesive Technologies, Duesseldorf (Germany); Henkel AG & Co KGaA, Duesseldorf (Germany)
  6. Adhesive Technologies, Henkel Corporation, Bridgewater, NJ (United States)
Publication Date:
Research Org.:
Brookhaven National Laboratory (BNL), Upton, NY (United States). Center for Functional Nanomaterials (CFN) and National Synchrotron Light Source II (NSLS-II)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES); Henkel Corporation
OSTI Identifier:
1614979
Alternate Identifier(s):
OSTI ID: 1605042
Report Number(s):
BNL-213842-2020-JAAM
Journal ID: ISSN 0021-8979; TRN: US2104970
Grant/Contract Number:  
SC0012704
Resource Type:
Accepted Manuscript
Journal Name:
Journal of Applied Physics
Additional Journal Information:
Journal Volume: 127; Journal Issue: 11; Journal ID: ISSN 0021-8979
Publisher:
American Institute of Physics (AIP)
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; X ray photon correlation spectroscopy; Differential scanning calorimetry

Citation Formats

Yavitt, Benjamin M., Salatto, Daniel, Huang, Zhixing, Koga, Yuto T., Endoh, Maya K., Wiegart, Lutz, Poeller, Sascha, Petrash, Stanislas, and Koga, Tadanori. Revealing nanoscale dynamics during an epoxy curing reaction with x-ray photon correlation spectroscopy. United States: N. p., 2020. Web. doi:10.1063/1.5141488.
Yavitt, Benjamin M., Salatto, Daniel, Huang, Zhixing, Koga, Yuto T., Endoh, Maya K., Wiegart, Lutz, Poeller, Sascha, Petrash, Stanislas, & Koga, Tadanori. Revealing nanoscale dynamics during an epoxy curing reaction with x-ray photon correlation spectroscopy. United States. https://doi.org/10.1063/1.5141488
Yavitt, Benjamin M., Salatto, Daniel, Huang, Zhixing, Koga, Yuto T., Endoh, Maya K., Wiegart, Lutz, Poeller, Sascha, Petrash, Stanislas, and Koga, Tadanori. Tue . "Revealing nanoscale dynamics during an epoxy curing reaction with x-ray photon correlation spectroscopy". United States. https://doi.org/10.1063/1.5141488. https://www.osti.gov/servlets/purl/1614979.
@article{osti_1614979,
title = {Revealing nanoscale dynamics during an epoxy curing reaction with x-ray photon correlation spectroscopy},
author = {Yavitt, Benjamin M. and Salatto, Daniel and Huang, Zhixing and Koga, Yuto T. and Endoh, Maya K. and Wiegart, Lutz and Poeller, Sascha and Petrash, Stanislas and Koga, Tadanori},
abstractNote = {In this work the evolution of nanoscale properties is measured during the thermally triggered curing of an industrial epoxy adhesive. We use x-ray photon correlation spectroscopy (XPCS) to track the progression of the curing reaction through the local dynamics of filler particles that reflect the formation of a thermoset network. Out-of-equilibrium dynamics are resolved through identification and analysis of the intensity– intensity autocorrelation functions obtained from XPCS. The characteristic time scale and local velocity of the filler is calculated as functions of time and temperature. We find that the dynamics speed up when approaching the curing temperature (Tcure), and decay rapidly once Tcure is reached. We compare the results from XPCS to conventional macroscale characterization by differential scanning calorimetry (DSC). The demonstration and implementation of nanoscale characterization of curing reactions by XPCS proves useful for future development and optimization of epoxy thermoset materials and other industrial adhesive systems.},
doi = {10.1063/1.5141488},
journal = {Journal of Applied Physics},
number = 11,
volume = 127,
place = {United States},
year = {2020},
month = {3}
}

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