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Title: Size effects in 3D–printed polymer–derived, zirconium diboride–reinforced ceramic composites

Abstract

Preceramic polymers are of interest for use in many manufacturing techniques such as injection molding, ceramic fiber infiltration, and additive manufacturing. However, off-gassing of low molecular weight oligomers occurs when these polymers cure, potentially leading to porosity in the cured part. Here to study how porosity and strength are affected by the size of the printed part, and the presence of a high surface area nano-scale filler, polycarbosilane (PCS) microrods of varying diameter were fabricated via direct ink writing (DIW), an additive manufacturing technique, with two ink formulations containing either zirconium diboride (ZrB2) alone, or ZrB2 and fumed alumina (FA). Sets of microrods were printed in a range of sizes by using print nozzles of 450, 634, 979, 1 346, or 1 702 μm in diameter, which were thermally cured, pyrolyzed to form ceramic composite microrods, and tested in 3-pt flexure. Porosity increased with increasing diameter, while failure strength decreased. For a given nozzle size, the microrods containing FA displayed lower porosity and higher strength (up to ~500 MPa) compared to the microrods containing only ZrB2. Weibull strength analysis was performed on each group of microrods and shows that the addition of FA increased Weibull modulus from 4.63 ± 1.56more » to 9.35 ± 0.601. In conjunction with optical microscopy, this analysis indicates two distinct flaw populations in the printed materials, porosity which arises during the curing step and cracking which arises during pyrolysis of the larger specimens.« less

Authors:
ORCiD logo [1];  [2]; ORCiD logo [2]
  1. Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States); Univ. of Tennessee, Knoxville, TN (United States)
  2. Univ. of Tennessee, Knoxville, TN (United States)
Publication Date:
Research Org.:
Kansas City Nuclear Security Campus (KCNSC), Kansas City, MO (United States)
Sponsoring Org.:
USDOE National Nuclear Security Administration (NNSA)
OSTI Identifier:
2282306
Grant/Contract Number:  
NA0002839
Resource Type:
Accepted Manuscript
Journal Name:
Journal of the American Ceramic Society
Additional Journal Information:
Journal Volume: 107; Journal Issue: 3; Journal ID: ISSN 0002-7820
Publisher:
American Ceramic Society
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; alumina; mechanical properties; precursors; pyrolysis

Citation Formats

Kemp, James William, Reed, Jesse Lynn, and Compton, Brett Gibson. Size effects in 3D–printed polymer–derived, zirconium diboride–reinforced ceramic composites. United States: N. p., 2023. Web. doi:10.1111/jace.19516.
Kemp, James William, Reed, Jesse Lynn, & Compton, Brett Gibson. Size effects in 3D–printed polymer–derived, zirconium diboride–reinforced ceramic composites. United States. https://doi.org/10.1111/jace.19516
Kemp, James William, Reed, Jesse Lynn, and Compton, Brett Gibson. Wed . "Size effects in 3D–printed polymer–derived, zirconium diboride–reinforced ceramic composites". United States. https://doi.org/10.1111/jace.19516.
@article{osti_2282306,
title = {Size effects in 3D–printed polymer–derived, zirconium diboride–reinforced ceramic composites},
author = {Kemp, James William and Reed, Jesse Lynn and Compton, Brett Gibson},
abstractNote = {Preceramic polymers are of interest for use in many manufacturing techniques such as injection molding, ceramic fiber infiltration, and additive manufacturing. However, off-gassing of low molecular weight oligomers occurs when these polymers cure, potentially leading to porosity in the cured part. Here to study how porosity and strength are affected by the size of the printed part, and the presence of a high surface area nano-scale filler, polycarbosilane (PCS) microrods of varying diameter were fabricated via direct ink writing (DIW), an additive manufacturing technique, with two ink formulations containing either zirconium diboride (ZrB2) alone, or ZrB2 and fumed alumina (FA). Sets of microrods were printed in a range of sizes by using print nozzles of 450, 634, 979, 1 346, or 1 702 μm in diameter, which were thermally cured, pyrolyzed to form ceramic composite microrods, and tested in 3-pt flexure. Porosity increased with increasing diameter, while failure strength decreased. For a given nozzle size, the microrods containing FA displayed lower porosity and higher strength (up to ~500 MPa) compared to the microrods containing only ZrB2. Weibull strength analysis was performed on each group of microrods and shows that the addition of FA increased Weibull modulus from 4.63 ± 1.56 to 9.35 ± 0.601. In conjunction with optical microscopy, this analysis indicates two distinct flaw populations in the printed materials, porosity which arises during the curing step and cracking which arises during pyrolysis of the larger specimens.},
doi = {10.1111/jace.19516},
journal = {Journal of the American Ceramic Society},
number = 3,
volume = 107,
place = {United States},
year = {Wed Oct 25 00:00:00 EDT 2023},
month = {Wed Oct 25 00:00:00 EDT 2023}
}

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