Tuning crosslinking of hybrid preceramic polymers in vat photopolymerization toward controlled ceramic yields

Kim, Sungjin; Biju, Catherine; Karunarathna, Menisha S.; Grimes, Niya Y.; Hmeidat, Nadim S.; Reyes-Zacarias, July; Agarwal, Shradha; Anisur Rahman, Md; Gilmer, Dustin B.; Compton, Brett G.; Bullock, Steve E.; Saito, Tomonori; Cramer, Corson L.

doi:10.1016/j.cej.2024.156585

Title: Tuning crosslinking of hybrid preceramic polymers in vat photopolymerization toward controlled ceramic yields

Journal Article · 10 October 2024 · Chemical Engineering Journal

DOI: https://doi.org/10.1016/j.cej.2024.156585 · OSTI ID:2474753

^[1]; Biju, Catherine ^[2]; Karunarathna, Menisha S. ^[3];

^[4];

^[3];

^[4]; Agarwal, Shradha ^[4];

^[3];

^[5]; Compton, Brett G. ^[4]; Bullock, Steve E. ^[3];

^[6];

^[3]

Univ. of New Mexico, Albuquerque, NM (United States); Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
Univ. of New Mexico, Albuquerque, NM (United States)
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
Univ. of Tennessee, Knoxville, TN (United States)
University of Tennessee-Oak Ridge Innovation Institute, Oak Ridge, TN (United States); Univ. of Tennessee, Knoxville, TN (United States)
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States); Univ. of Tennessee, Knoxville, TN (United States); University of Tennessee-Oak Ridge Innovation Institute, Oak Ridge, TN (United States)

Control of preceramic polymer crosslinking for UV-curable processing is essential for fine 3D printing with high ceramic conversion for sustainable polymer-derived ceramics (PDC) engineering. While various factors influencing ceramic yield have been studied, the systematic exploration of the relationship between crosslinking and ceramic yield, especially when crosslinking increases volatile elements, remains open for further investigation. This study addresses this gap by utilizing vat photopolymerization (VP) additive manufacturing (AM) as a versatile platform for controlling preceramic crosslinking and ceramic yield. By rationally designing and tuning the photochemical crosslinking through digital light processing (DLP), we demonstrate that the ceramic yield can be enhanced from 64% to over 86%, even with added volatile elements. We reveal that the post-pyrolysis ceramic yield can be closely correlated with the pre-pyrolysis crosslinking of the preceramic network represented by its stiffness. This correlation thereby suggests a fast, energy-efficient, non-destructive methodology to predict and improve ceramic yield. Combined with these findings, our one-pot thiol-ene hybridization of polycarbosilane and polycarbosiloxane via DLP offers an exemplary method to generate hybrid preceramic polymers with tailored material properties toward target applications, and potentially even higher ceramic yields. This study thus contributes to achieving better resource- and energy-efficient preceramic polymer and PDC processing routes toward sustainable, advanced organic–inorganic materials manufacturing.

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Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

Sponsoring Organization:: USDOE

Grant/Contract Number:: AC05-00OR22725

OSTI ID:: 2474753

Journal Information:: Chemical Engineering Journal, Journal Name: Chemical Engineering Journal Vol. 499; ISSN 1385-8947

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
Ceramic yield
Crosslinking
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Polymer-derived ceramics
Preceramic polymer
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Title: Tuning crosslinking of hybrid preceramic polymers in vat photopolymerization toward controlled ceramic yields

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