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Title: Structural Dynamics in UV Curable Resins Resolved by In Situ 3D Printing X-ray Photon Correlation Spectroscopy

Abstract

Additive manufacturing (AM) is a promising technique to rapidly produce polymeric materials into complex 3-dimensional (3D) geometries. While AM is widespread and relevant for a range of applications, implementation in industry has outpaced our fundamental understanding of polymer dynamics and structure development during the printing process. Characterization and quantification of such dynamics is necessary to optimize final material properties and design future materials and processes for 3D printing. Here, we utilize X-ray photon correlation spectroscopy (XPCS) to measure spatial and time-resolved, out-of-equilibrium dynamics during direct ink write (DIW) 3D printing. Specifically, we investigate the progression of structural dynamics in a dual cure (UV/thermal) nanocomposite during and directly after printing. As the filament is printed and cured in situ, the relaxation processes of the cross-linking network are measured through the dynamics of inorganic filler particles. The characteristic relaxation time of the dynamics is calculated through the intensity–intensity autocorrelation function g2 and directly correlated to the printing process parameters, such as printhead velocity and UV light intensity. The time-resolved evolution of nanoscale dynamics follows a power-law dependence as the filament is cured. Additionally, bulk rheological characterizations reveal the macroscopic solidification of the resin, providing correlation of material properties across a wide rangemore » of length and time scales. Overall, the measurement of multiscale, out-of-equilibrium dynamics provides insight into the development of structure in polymer nanocomposite filaments during 3D printing and is used to further understand the influence of such parameters on the AM process.« less

Authors:
ORCiD logo [1];  [2];  [3];  [3]; ORCiD logo [3];  [4];  [5]; ORCiD logo [3]
  1. Stony Brook Univ., NY (United States); Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)
  2. Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)
  3. Stony Brook Univ., NY (United States)
  4. Adhesive Technologies, Duesseldorf (Germany)
  5. Adhesive Technologies, Henkel Corporation, Bridgewater, NJ (United States)
Publication Date:
Research Org.:
Brookhaven National Lab. (BNL), Upton, NY (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
OSTI Identifier:
1716764
Report Number(s):
BNL-220612-2020-JAAM
Journal ID: ISSN 2637-6105
Grant/Contract Number:  
SC0012704
Resource Type:
Accepted Manuscript
Journal Name:
ACS Applied Polymer Materials
Additional Journal Information:
Journal Volume: 2; Journal Issue: 9; Journal ID: ISSN 2637-6105
Publisher:
ACS Publications
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; X-ray photon correlation spectroscopy; 3D printed thermoset resins; UV curing; out-of-equilibrium dynamics; rheology; spatial

Citation Formats

Yavitt, Benjamin M., Wiegart, Lutz, Salatto, Daniel, Huang, Zhixing, Endoh, Maya K., Poeller, Sascha, Petrash, Stanislas, and Koga, Tadanori. Structural Dynamics in UV Curable Resins Resolved by In Situ 3D Printing X-ray Photon Correlation Spectroscopy. United States: N. p., 2020. Web. https://doi.org/10.1021/acsapm.0c00716.
Yavitt, Benjamin M., Wiegart, Lutz, Salatto, Daniel, Huang, Zhixing, Endoh, Maya K., Poeller, Sascha, Petrash, Stanislas, & Koga, Tadanori. Structural Dynamics in UV Curable Resins Resolved by In Situ 3D Printing X-ray Photon Correlation Spectroscopy. United States. https://doi.org/10.1021/acsapm.0c00716
Yavitt, Benjamin M., Wiegart, Lutz, Salatto, Daniel, Huang, Zhixing, Endoh, Maya K., Poeller, Sascha, Petrash, Stanislas, and Koga, Tadanori. Mon . "Structural Dynamics in UV Curable Resins Resolved by In Situ 3D Printing X-ray Photon Correlation Spectroscopy". United States. https://doi.org/10.1021/acsapm.0c00716. https://www.osti.gov/servlets/purl/1716764.
@article{osti_1716764,
title = {Structural Dynamics in UV Curable Resins Resolved by In Situ 3D Printing X-ray Photon Correlation Spectroscopy},
author = {Yavitt, Benjamin M. and Wiegart, Lutz and Salatto, Daniel and Huang, Zhixing and Endoh, Maya K. and Poeller, Sascha and Petrash, Stanislas and Koga, Tadanori},
abstractNote = {Additive manufacturing (AM) is a promising technique to rapidly produce polymeric materials into complex 3-dimensional (3D) geometries. While AM is widespread and relevant for a range of applications, implementation in industry has outpaced our fundamental understanding of polymer dynamics and structure development during the printing process. Characterization and quantification of such dynamics is necessary to optimize final material properties and design future materials and processes for 3D printing. Here, we utilize X-ray photon correlation spectroscopy (XPCS) to measure spatial and time-resolved, out-of-equilibrium dynamics during direct ink write (DIW) 3D printing. Specifically, we investigate the progression of structural dynamics in a dual cure (UV/thermal) nanocomposite during and directly after printing. As the filament is printed and cured in situ, the relaxation processes of the cross-linking network are measured through the dynamics of inorganic filler particles. The characteristic relaxation time of the dynamics is calculated through the intensity–intensity autocorrelation function g2 and directly correlated to the printing process parameters, such as printhead velocity and UV light intensity. The time-resolved evolution of nanoscale dynamics follows a power-law dependence as the filament is cured. Additionally, bulk rheological characterizations reveal the macroscopic solidification of the resin, providing correlation of material properties across a wide range of length and time scales. Overall, the measurement of multiscale, out-of-equilibrium dynamics provides insight into the development of structure in polymer nanocomposite filaments during 3D printing and is used to further understand the influence of such parameters on the AM process.},
doi = {10.1021/acsapm.0c00716},
journal = {ACS Applied Polymer Materials},
number = 9,
volume = 2,
place = {United States},
year = {2020},
month = {7}
}

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