A rapid FIB-notch technique for characterizing the internal morphology of high-performance fibers

Stockdale, Taylor A.; Strawhecker, Kenneth E.; Sandoz-Rosado, Emil; Wetzel, Eric D.

doi:10.1016/j.matlet.2016.04.082

Cited by 21 publications

(24 citation statements)

References 15 publications

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“…This creates a flat interior surface of the fiber, with minimal damage to fiber meso/nanostructure on which experiments may be performed. Stockdale et al discuss the details of the experimental technique as well as a detailed look at the preserved microstructure in the shear plane in their article.…”

Section: Methodsmentioning

confidence: 99%

Nanoscale interfibrillar adhesion in UHMWPE fibers

McDaniel

Strawhecker

Deitzel

et al. 2017

J Polym Sci B Polym Phys

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The goal of this research is to quantify the fibrillar adhesive energy in ultra-high molecular weight polyethylene fibers, characteristic of nanoscale fibril interactions. Quantification of these energies is vital to the understanding of fibrillar deformation mechanisms that have been shown to play an important role in fiber performance. This is achieved through the development and implementation of a nanosplitting technique developed through the use of AFM-enabled nanoindentation. This technique allows the quantification of nanoscale adhesive energies through careful monitoring of load and unload curves as well as examination of the residual split through high-resolution AFM images. Results indicate that the average nanoscale fibril adhesive energy is over 3 times larger than the energy expected from van der Waals interactions alone. This indicates that a significant degree of physical interactions exist between fibrils, beyond van der Waals interactions, in the form of tie-molecules, fibrillar network junctions, and bridging lamellar crystals.

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Section: Methodsmentioning

confidence: 99%

Nanoscale interfibrillar adhesion in UHMWPE fibers

McDaniel

Strawhecker

Deitzel

et al. 2017

J Polym Sci B Polym Phys

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“…In order to prepare the samples for these morphology studies, a novel FIB-notch technique was employed which has been detailed elsewhere [ 14 ]. Once the FIB-notch technique is used to expose an internal surface for scanning, the samples are mounted on a double-sided adhesive for AFM imaging.…”

Section: Methodsmentioning

confidence: 99%

“…Direct SEM is not particularly effective on nonconducting high-performance fibers like UHMWPE and Kevlar; a metal coating must be applied to the fibers to prevent melting by the electron beam, and the technique only reports topographical information. Finally, TEM, while able to provide spatial crystalline orientation, requires microtoming specimens to thicknesses of tens of nanometers which is difficult and potentially alters the microstructure due to violent cross sectioning [ 14 ].…”

Section: Introductionmentioning

confidence: 99%

“…Prior work has established high-resolution, transverse-stiffness AFM and careful shear notch sample preparation as a method for revealing internal fiber morphology that is rich with information [ 14 – 18 ]. This method is also known as the “FIB-notch” technique since a focused ion beam, FIB, is used to cut opposing notches along a fiber to induce shear failure along an internal plane via minimal applied load.…”

Section: Introductionmentioning

confidence: 99%

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Quantifying High-Performance Material Microstructure Using Nanomechanical Tools with Visual and Frequency Analysis

2018

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High-performance materials like ballistic fibers have remarkable mechanical properties owing to specific patterns of organization ranging from the molecular scale, to the micro scale and macro scale. Understanding these strategies for material organization is critical to improving the mechanical properties of these high-performance materials. In this work, atomic force microscopy (AFM) was used to detect changes in material composition at an extremely high resolution with transverse-stiffness scanning. New methods for direct quantification of material morphology were developed, and applied as an example to these AFM scans, although these methods can be applied to any spatially-resolved scans. These techniques were used to delineate between subtle morphological differences in commercial ultra-high-molecular-weight polyethylene (UHMWPE) fibers that have different processing conditions and mechanical properties as well as quantify morphology in commercial Kevlar®, a high-performance material with an entirely different organization strategy. Both frequency analysis and visual processing methods were used to systematically quantify the microstructure of the fiber samples in this study. These techniques are the first step in establishing structure-property relationships that can be used to inform synthesis and processing techniques to achieve desired morphologies, and thus superior mechanical performance.

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“…4 show the amplitude versus distance and the phase versus distance spectra, respectively. These are shown for both the spin-cast PS (Bruker) and the UHMWPE (prepared using a focused-ion-beam notching technique) [4]. What should be noted from these plots is the region of operation for the multi-frequency technique, in specific, the bottom region of the first mode amplitude plot is the imaging amplitude setpoint (1 V).…”

Section: Experimental Design Materials and Methodsmentioning

confidence: 99%

Background data for modulus mapping high-performance polyethylene fiber morphologies

et al. 2017

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The data included here provides a basis for understanding “Interior morphology of high-performance polyethylene fibers revealed by modulus mapping” (K.E. Strawhecker, E.J. Sandoz-Rosado, T.A. Stockdale, E.D. Laird, 2016) [1], in specific: the multi-frequency (AMFM) atomic force microscopy technique and its application to ultra-high-molecular-weight Polyethylene (UHMWPE) fibers. Furthermore, the data suggests why the Hertzian contact mechanics model can be used within the framework of AMFM theory, simple harmonic oscillator theory, and contact mechanics. The framework is first laid out followed by data showing cantilever dynamics, force-distance spectra in AC mode, and force-distance in contact mode using Polystyrene reference and UHMWPE. Finally topography and frequency shift (stiffness) maps are presented to show the cases where elastic versus plastic deformation may have occurred.

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A rapid FIB-notch technique for characterizing the internal morphology of high-performance fibers

Cited by 21 publications

References 15 publications

Nanoscale interfibrillar adhesion in UHMWPE fibers

Nanoscale interfibrillar adhesion in UHMWPE fibers

Quantifying High-Performance Material Microstructure Using Nanomechanical Tools with Visual and Frequency Analysis

Background data for modulus mapping high-performance polyethylene fiber morphologies

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