Revealing filler morphology in 3D-printed thermoset nanocomposites by scanning microbeam X-ray scattering

Edward B. Trigg; Nadim S. Hmeidat; Louisa M. Smieska; Arthur R. Woll; Brett G. Compton; Hilmar Koerner

doi:10.1016/j.addma.2020.101729

Revealing filler morphology in 3D-printed thermoset nanocomposites by scanning microbeam X-ray scattering

Edward B. Trigg
, Nadim S. Hmeidat
, Louisa M. Smieska
, Arthur R. Woll
, Brett G. Compton
, Hilmar Koerner

Research output: Contribution to journal › Article › peer-review

25 Scopus citations

Abstract

Room temperature direct-ink-write printing of epoxy-nanoclay-carbon fiber composites produces parts with high stiffness and strength. Establishing clear relationships between print parameters, filler orientation, and properties is difficult, in part owing to challenges in characterization. Here, we perform scanning microbeam X-ray scattering with 5 micrometer spatial resolution on cross-sections of printed parts with (a) epoxy-nanoclay composite and (b) epoxy-nanoclay-carbon fiber reinforced composite. The nanoclay morphology is directly visualized, illuminating the road geometry with far greater clarity than other techniques. Near the boundary of each road, the nanoclay platelets are preferentially oriented coplanar with the road boundary. Shear alignment within the nozzle during extrusion, and road-to-road shear upon deposition are two proposed factors leading to this orientation. In the sample containing carbon fiber, wide angle X-ray diffraction enables the mapping and visualization of the fibers directly onto the road geometry. The carbon fiber does not significantly affect the nanoclay morphology. Finally, from the small angle X-ray scattering map, we qualitatively reproduce a polarized optical microscope image, revealing that optical microscopy is capable of visualizing the large-scale road structure in these epoxy-nanoclay systems.

Original language	English
Article number	101729
Journal	Additive Manufacturing
Volume	37
DOIs	https://doi.org/10.1016/j.addma.2020.101729
State	Published - Jan 2021
Externally published	Yes

Funding

This research was performed while E.B.T. held an NRC Research Associateship award at the Air Force Research Laboratory (Wright-Patterson Air Force Base, Ohio). This project received funding from AFOSR under Dr. Jaimie Tiley and Ming-Jen Pan under the Low Density Portfolio #17RXCOR436. N.S.H and B.G.C would like to acknowledge funding from NSF under grant no. CMMI-1825815, and Honeywell Federal Manufacturing and Technologies through Contract DE-NA0002839, administrated by Dr. Jamie Messman, Mr. Steven Patterson, and Dr. Eric Eastwood. This work is based upon research conducted at the Materials Solutions Network at CHESS (MSN-C) which is supported by the Air Force Research Laboratory under award FA8650-19-2-5220. This research was performed while E.B.T. held an NRC Research Associateship award at the Air Force Research Laboratory (Wright-Patterson Air Force Base, Ohio). This project received funding from AFOSR under Dr. Jaimie Tiley and Ming-Jen Pan under the Low Density Portfolio #17RXCOR436 . N.S.H and B.G.C would like to acknowledge funding from NSF under grant no. CMMI-1825815 , and Honeywell Federal Manufacturing and Technologies through Contract DE-NA0002839 , administrated by Dr. Jamie Messman, Mr. Steven Patterson, and Dr. Eric Eastwood. This work is based upon research conducted at the Materials Solutions Network at CHESS (MSN-C) which is supported by the Air Force Research Laboratory under award FA8650-19-2-5220 .

Keywords

Composite
Direct ink write
Epoxy
Scanning microbeam X-ray scattering

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10.1016/j.addma.2020.101729

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title = "Revealing filler morphology in 3D-printed thermoset nanocomposites by scanning microbeam X-ray scattering",

abstract = "Room temperature direct-ink-write printing of epoxy-nanoclay-carbon fiber composites produces parts with high stiffness and strength. Establishing clear relationships between print parameters, filler orientation, and properties is difficult, in part owing to challenges in characterization. Here, we perform scanning microbeam X-ray scattering with 5 micrometer spatial resolution on cross-sections of printed parts with (a) epoxy-nanoclay composite and (b) epoxy-nanoclay-carbon fiber reinforced composite. The nanoclay morphology is directly visualized, illuminating the road geometry with far greater clarity than other techniques. Near the boundary of each road, the nanoclay platelets are preferentially oriented coplanar with the road boundary. Shear alignment within the nozzle during extrusion, and road-to-road shear upon deposition are two proposed factors leading to this orientation. In the sample containing carbon fiber, wide angle X-ray diffraction enables the mapping and visualization of the fibers directly onto the road geometry. The carbon fiber does not significantly affect the nanoclay morphology. Finally, from the small angle X-ray scattering map, we qualitatively reproduce a polarized optical microscope image, revealing that optical microscopy is capable of visualizing the large-scale road structure in these epoxy-nanoclay systems.",

keywords = "Composite, Direct ink write, Epoxy, Scanning microbeam X-ray scattering",

author = "Trigg, \{Edward B.\} and Hmeidat, \{Nadim S.\} and Smieska, \{Louisa M.\} and Woll, \{Arthur R.\} and Compton, \{Brett G.\} and Hilmar Koerner",

note = "Publisher Copyright: {\textcopyright} 2020",

year = "2021",

month = jan,

doi = "10.1016/j.addma.2020.101729",

language = "English",

volume = "37",

journal = "Additive Manufacturing",

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AU - Trigg, Edward B.

AU - Hmeidat, Nadim S.

AU - Smieska, Louisa M.

AU - Woll, Arthur R.

AU - Compton, Brett G.

AU - Koerner, Hilmar

PY - 2021/1

Y1 - 2021/1

N2 - Room temperature direct-ink-write printing of epoxy-nanoclay-carbon fiber composites produces parts with high stiffness and strength. Establishing clear relationships between print parameters, filler orientation, and properties is difficult, in part owing to challenges in characterization. Here, we perform scanning microbeam X-ray scattering with 5 micrometer spatial resolution on cross-sections of printed parts with (a) epoxy-nanoclay composite and (b) epoxy-nanoclay-carbon fiber reinforced composite. The nanoclay morphology is directly visualized, illuminating the road geometry with far greater clarity than other techniques. Near the boundary of each road, the nanoclay platelets are preferentially oriented coplanar with the road boundary. Shear alignment within the nozzle during extrusion, and road-to-road shear upon deposition are two proposed factors leading to this orientation. In the sample containing carbon fiber, wide angle X-ray diffraction enables the mapping and visualization of the fibers directly onto the road geometry. The carbon fiber does not significantly affect the nanoclay morphology. Finally, from the small angle X-ray scattering map, we qualitatively reproduce a polarized optical microscope image, revealing that optical microscopy is capable of visualizing the large-scale road structure in these epoxy-nanoclay systems.

AB - Room temperature direct-ink-write printing of epoxy-nanoclay-carbon fiber composites produces parts with high stiffness and strength. Establishing clear relationships between print parameters, filler orientation, and properties is difficult, in part owing to challenges in characterization. Here, we perform scanning microbeam X-ray scattering with 5 micrometer spatial resolution on cross-sections of printed parts with (a) epoxy-nanoclay composite and (b) epoxy-nanoclay-carbon fiber reinforced composite. The nanoclay morphology is directly visualized, illuminating the road geometry with far greater clarity than other techniques. Near the boundary of each road, the nanoclay platelets are preferentially oriented coplanar with the road boundary. Shear alignment within the nozzle during extrusion, and road-to-road shear upon deposition are two proposed factors leading to this orientation. In the sample containing carbon fiber, wide angle X-ray diffraction enables the mapping and visualization of the fibers directly onto the road geometry. The carbon fiber does not significantly affect the nanoclay morphology. Finally, from the small angle X-ray scattering map, we qualitatively reproduce a polarized optical microscope image, revealing that optical microscopy is capable of visualizing the large-scale road structure in these epoxy-nanoclay systems.

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KW - Epoxy

KW - Scanning microbeam X-ray scattering

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DO - 10.1016/j.addma.2020.101729

M3 - Article

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JO - Additive Manufacturing

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ER -

Revealing filler morphology in 3D-printed thermoset nanocomposites by scanning microbeam X-ray scattering

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