Ink-substrate interactions during 3D printing revealed by time-resolved coherent X-ray scattering

Arango, M. Torres; Zhang, Y.; Zhao, Chonghang; Li, R.; Doerk, Gregory S.; Nykypanchuk, Dmytro; Chen-Wiegart, Y-c. K.; Fluerasu, Andrei; Wiegart, Lutz

doi:10.1016/j.mtphys.2020.100220

Cited by 13 publications

(25 citation statements)

References 55 publications

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“…In situ XPCS during 3D printing was recently demonstrated by Johnson et al and Torres Arango et al , Here, we aim to implement such techniques to resolve behavior of 3D printed polymer–filler composites during industrially relevant operations. Specifically, we investigate an industrial dual cure acrylate/epoxy thermoset resin during and directly after printing.…”

Section: Introductionmentioning

confidence: 99%

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

Yavitt

Wiegart

Salatto

et al. 2020

ACS Appl. Polym. Mater.

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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 g 2 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. Bulk rheological characterizations reveal the macroscopic solidification of the resin, providing correlation of material properties across a wide range of length and time scales. 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.

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Section: Introductionmentioning

confidence: 99%

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

Yavitt

Wiegart

Salatto

et al. 2020

ACS Appl. Polym. Mater.

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“…In a study by Johnson et al, thermoset nanocomposites were monitored using X-Ray photon correlation spectroscopy (XPCS). [121] This technique explores the effects that print and substrate parameters have on the morphology and dynamics used in the direct write process of thermosetting nanocomposite or conductive inks [122] . During experiments, filaments were deposited across the X-ray beam path, with the print head moving in an x-translation direction (Figure 13).…”

Section: Real Time Monitoring For Process Controlmentioning

confidence: 99%

“…[ 121 ] This technique explores the effects that print and substrate parameters have on the morphology and dynamics used in the direct write process of thermosetting nanocomposite or conductive inks. [ 122 ] During experiments, filaments were deposited across the X‐ray beam path, with the print head moving in an x‐translation direction ( Figure ). Once the filament has been deposited, there is no movement outside of the viscoelastic drag of the material that is an unavoidable part of the printing process.…”

Section: Am Enabling Nanocomposite Morphology Control | Nanocomposite...mentioning

confidence: 99%

Best of Both Worlds: Synergistically Derived Material Properties via Additive Manufacturing of Nanocomposites

Carrola

Asadi

Zhang

et al. 2021

Adv Funct Materials

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With an exponential rise in the popularity and availability of additive manufacturing (AM), a large focus has been directed toward research in this topic's movement, while trying to distinguish themselves from similar works by simply adding nanomaterials to their process. Though nanomaterials can add impressive properties to nanocomposites (NCs), there are expansive amounts of opportunities that are left unexplored by simply combining AM with NCs without discovering synergistic effects and novel emerging material properties that are not possible by each of these alone. Cooperative, evolving properties of NCs in AM can be investigated at the processing, morphological, and architectural levels. Each of these categories are studied as a function of the amplifying relationship between nanomaterials and AM, with each showing the systematically selected material and method to advance the material performance, explore emergent properties, as well as improve the AM process itself. Innovative, advanced materials are key to faster development cycles in disruptive technologies for bioengineering, defense, and transportation sectors. This is only possible by focusing on synergism and amplification within additive manufacturing of nanocomposites.

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“…Additive manufacturing techniques are central to important advances across multiple technological fields. , 3D-printed ceramics are commonly sought for the outstanding semiconducting, , catalytic, , structural, − and biocompatible , properties of these material systems for sensing, biomedicine, waste management, energy, and extreme environment applications. ,, Continuous filament direct ink writing (DIW), in particular, offers great material/microstructural design freedom, suitable for a wide range of ink viscosities (10 2 –10 6 Pa·s) and print resolution (micrometers to millimeters) . Inherent to the printing process are the out-of-equilibrium shear and relaxation stages influencing the inks as they flow through the nozzle, get deposited as filaments, and consecutively recover. − Further relaxation and rearrangement of the microstructure across various length scales occur as drying or more generally curing progresses, commonly resulting in volumetric contraction and sometimes cracking, delamination, or poor filament–filament or filament–substrate adhesion. Being able to follow and spatially resolve such evolution in terms of the microstructural changes (including their characteristic time- and length-scales and orientation with respect to a printing system of reference) is key for understanding and addressing processing specific mechanisms which might be related to defects and may be exploited to improve the components’ performance (mechanical, electrical, etc.).…”

Section: Introductionmentioning

confidence: 99%

“…Here, “solidification” is used as a collective term for all processes that proceed after the filament deposition and that transform the extruded, shear-thinned, sol–gel into an elastic solid. However, the associated transformations and underlying mechanisms during such processes remain unclear, mainly due to the technical difficulties in studying such fast and spatially heterogeneous transient states with sufficient temporal and spatial resolution , under operando conditions. Recent works on viscoelastic colloidal inks used X-ray photon correlation spectroscopy (XPCS) to provide information on the out-of-equilibrium pathways associated with printing, , showing that such systems undergo characteristic relaxation–time profiles upon extrusion and recovery.…”

Section: Introductionmentioning

confidence: 99%

In-Operando Study of Shape Retention and Microstructure Development in a Hydrolyzing Sol–Gel Ink during 3D-Printing

Arango

Zhang

et al. 2020

ACS Appl. Mater. Interfaces

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3D printing of amorphous and crystalline ceramics is of paramount importance for the fabrication of a wide range of devices with applications across different technology fields. Printed ceramics are remarkably enabled by the sol–gel synthesis method in conjunction with continuous filament direct ink writing. During printing, multiple processes contribute to the evolution of inks including shape retention, chemical conversion, solidification, and microstructure formation. Traditionally, depending on the ink composition and printing environment, several mechanisms have been associated with the shape retention and solidification of 3D printed structures: gelation, rapid solvent evaporation, energy-driven phase transformation, and chemical-driven phase transformation. Understanding the fundamental differences between these mechanisms becomes key since they strongly influence the spatiotemporal evolution of the materials, as the out-of-equilibrium processes inherent to the extrusion, relaxation, and solidification of printed materials have significant effects on the materials properties. In this work, we investigate the shape retention mechanism and the hydrolysis-induced material conversion and microstructure formation during the 3D printing of a water reactive sol–gel ink that transforms into titanium dioxide-based ceramic. This study aims at identifying characteristic mechanisms associated with the material transformation, establishing connections between the microstructure development and the timescales associated with solidification under operando 3D-printing conditions. The investigation of this material’s out-of-equilibrium pathways under processing conditions is enabled by time-resolved coherent X-ray scattering, providing simultaneous access to temporospatially resolved microstructural and dynamics information. Furthermore, we explore X-ray speckle tracking as a tool to resolve deformations of the microstructure in a printed filament associated with the deposition of consecutive filaments. Through this work, we aim at providing a fundamental understanding of the relationships behind these transformative processes in 3D printing and their timescales as the basis for achieving unprecedented control over printed materials microstructure.

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Ink-substrate interactions during 3D printing revealed by time-resolved coherent X-ray scattering

Cited by 13 publications

References 55 publications

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

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

Best of Both Worlds: Synergistically Derived Material Properties via Additive Manufacturing of Nanocomposites

In-Operando Study of Shape Retention and Microstructure Development in a Hydrolyzing Sol–Gel Ink during 3D-Printing

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