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Philosophical Transactions of the Royal Society

As classical 1D nanoscale structures, carbon nanotubes (CNTs) possess remarkable mechanical, electrical, thermal, and optical properties. In the past several years, considerable attention has been paid to the use of CNTs as building blocks for novel high-performance materials. In this way, the production of macroscopic architectures based on assembled CNTs with controlled orientation and configurations is an important step towards their application. So far, various forms of macroscale CNT assemblies have been produced, such as 1D CNT fibers, 2D CNT films/sheets, and 3D aligned CNT arrays or foams. These macroarchitectures, depending on the manner in which they are assembled, display a variety of fascinating features that cannot be achieved using conventional materials. This review provides an overview of various macroscopic CNT assemblies, with a focus on their preparation and mechanical properties as well as their potential applications in practical fields.

Macroscopic Carbon Nanotube Assemblies: Preparation, Properties, and Potential Applications

A paradigm shift has emerged over the last decade pointing to an exciting research area dealing with the harnessing of elastic structural instabilities for ‘smart’ purposes in a variety of venues. Among the different types of unstable responses, buckling is a phenomenon that has been known for centuries, and yet it is generally avoided through special design modifications. Increasing interest in the design of smart devices and mechanical systems has identified buckling and postbuckling response as a favorable behavior. The objective of this topical review is to showcase the recent advances in buckling-induced smart applications and to explain why buckling responses have certain advantages and are especially suitable for these particular applications. Interesting prototypes in terms of structural forms and material uses associated with these applications are summarized. Finally, this review identifies potential research avenues and emerging trends for using buckling and other elastic instabilities for future innovations.

https://iopscience.iop.org/article/10.1088/0964-1726/24/6/063001/pdf

Buckling-induced smart applications: recent advances and trends

The design and fabrication of ultrathin polymer layers are of increasing importance because of the rapid development of nanoscience and nanotechnology. Confined, two-dimensional crystallization of polymers presents challenges and opportunities due to the long-chain, covalently bonded nature of the macromolecule. Using an innovative layer-multiplying coextrusion process to obtain assemblies with thousands of polymer nanolayers, we discovered a morphology that emerges as confined polyethylene oxide (PEO) layers are made progressively thinner. When the thickness is confined to 20 nanometers, the PEO crystallizes as single, high-aspect-ratio lamellae that resemble single crystals. Unexpectedly, the crystallization habit imparts two orders of magnitude reduction in the gas permeability.

High gas barrier from confined crystallization of polyethylene oxide in nanolayer assemblies

Although indentation experiments have long been used to measure the hardness and Young's modulus, the utility of this technique in analyzing the complete elastic–plastic response of materials under contact loading has only been realized in the past few years – mostly due to recent advances in testing equipment and analysis protocols. This paper provides a timely review of the recent progress made in this respect in extracting meaningful indentation stress–strain curves from the raw datasets measured in instrumented spherical nanoindentation experiments. These indentation stress–strain curves have produced highly reliable estimates of the indentation modulus and the indentation yield strength in the sample, as well as certain aspects of their post-yield behavior, and have been critically validated through numerical simulations using finite element models as well as direct in situ scanning electron microscopy (SEM) measurements on micro-pillars. Much of this recent progress was made possible through the introduction of a new measure of indentation strain and the development of new protocols to locate the effective zero-point of initial contact between the indenter and the sample in the measured datasets. This has led to an important key advance in this field where it is now possible to reliably identify and analyze the initial loading segment in the indentation experiments. Major advances have also been made in correlating the local mechanical response measured in nanoindentation with the local measurements of structure at the indentation site using complementary techniques. For example, it has been shown that the combined use of Orientation Imaging Microscopy (OIM, using Electron BackScattered Diffraction (EBSD)) and nanoindentation on polycrystalline metallic samples can yield important information on the orientation dependence of indentation yield stress, which can in turn be used to estimate percentage increase in the local slip resistance in deformed samples. The same methods have been used successfully to probe the intrinsic role of grain boundaries in the overall mechanical deformation of the sample. More recently, these protocols have been extended to characterize local mechanical property changes in the damaged layers in ion-irradiated metals. Similarly, the combined use of Raman spectroscopy and nanoindentation on samples of mouse bone has revealed tissue-level correlations between the mineral content at the indentation site and the associated local mechanical properties. The new protocols have also provided several new insights into the buckling response in dense carbon nanotube (CNT) brushes. These and other recent successful applications of nanoindentation are expected to provide the critically needed information for the maturation of physics-based multiscale models for the mechanical behavior of most advanced materials. In this paper, we review these latest developments and identify the future challenges that lie ahead.

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Spherical nanoindentation stress–strain curves

Uniaxial compression studies are performed on 50-µm-diameter bundles of nominally vertical, intertwined carbon nanotubes grown via chemical vapor deposition from a photolithographically defined catalyst. The inhomogeneous microstructure is examined, demonstrating density and tube orientation gradients, believed to play a role in the unique periodic buckling deformation mechanism. Through in situ uniaxial compression experiments it is discovered that the characteristic bottom-to-top sequential buckling proceeds by first nucleating on the bundle surface and subsequently propagating laterally through the bundle, gradually collapsing the entire structure. The effects of strain rate are explored, and storage and loss stiffnesses are analyzed in the context of energy dissipation.

In situ Mechanical Testing Reveals Periodic Buckle Nucleation and Propagation in Carbon Nanotube Bundles

The inherently fragile nature of ultrathin polymer films presents difficulties to the measurement of their mechanical properties, which are of interest in packaging, electronics, separations, and other manufacturing fields. More fundamentally, the direct measurement of ultrathin film mechanical properties is necessary for understanding changes in intrinsic material properties at reduced size scales, for example, when the film thickness alters the equilibrium configuration of the polymer chains. We introduce a method for ultrathin film tensile testing that stretches a two-dimensionally macroscopic, yet nanoscopically thin, polymer film on the surface of water. For polystyrene films, we observe a precipitous decrease in mechanical properties (Young’s modulus, strain at failure, and nominal stress at failure) for film thicknesses down to 15 nm, less than the characteristic size of an individual polymer chain, yielding new insights into the changes in polymer chain entanglements in confined states.

Directly Measuring the Complete Stress–Strain Response of Ultrathin Polymer Films

We carry out axisymmetric, finite deformation finite element analyses of the uniaxial compression of cylindrical bundles of vertically aligned carbon nanotubes (VACNTs) firmly attached to a Si substrate. A compressible elastic–viscoplastic constitutive relation with a piecewise, linear hardening–softening–hardening flow strength is used to model the material. Calculations are performed for VACNTs both with uniform properties and with axially graded properties. We show that, with uniform properties, sequential buckling initiates at the substrate and propagates away from it, in agreement with previous experimental findings. We investigate the dependence of the magnitude and wavelength of the buckles on characteristics of the function defining the flow strength. When a property gradient giving a more compliant response at the end opposite to the substrate is specified, we find that sequential buckling initiates at that end and propagates toward the substrate. Results of the analyses are compared with the experimental observations and capture many of the experimentally obtained stress–strain and morphological features. The proposed model serves as a promising foundation for capturing the underlying energy absorption mechanisms in these systems. Comparison of the model predictions with the experimental results also suggests directions for model improvement.

Analysis of uniaxial compression of vertically aligned carbon nanotubes

The cavitation rheology technique extracts soft materials mechanical properties through pressure-monitored fluid injection. Properties are calculated from the system's response at a critical pressure that is governed by either elasticity or fracture (or both); however previous elementary analysis has not been capable of accurately determining which mechanism is dominant. We combine analyses of both mechanisms in order to determine how the full system thermodynamics, including far-field compliance, dictate whether a bubble in an elastomeric solid will grow through either reversible or irreversible deformations. Applying these analyses to experimental data, we demonstrate the sensitivity of cavitation rheology to microstructural variation via a co-dependence between modulus and fracture energy.

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Elastic cavitation and fracture via injection

A generalized Rayleigh–Plesset-type bubble dynamics model with a damage mechanism is developed for cavitation and damage of soft materials by focused ultrasound bursts. This study is linked to recent experimental observations in tissue-mimicking polyacrylamide and agar gel phantoms subjected to bursts of a kind being considered specifically for lithotripsy. These show bubble activation at multiple sites during the initial pulses. More cavities appear continuously through the course of the observations, similar to what is deduced in pig kidney tissues in shock-wave lithotripsy. Two different material models are used to represent the distinct properties of the two gel materials. The polyacrylamide gel is represented with a neo-Hookean elastic model and damaged based upon a maximum-strain criterion; the agar gel is represented with a strain-hardening Fung model and damaged according to the strain-energy-based Griffith's fracture criterion. Estimates based upon independently determined elasticity and viscosity of the two gel materials suggest that bubble confinement should be sufficient to prevent damage in the gels, and presumably injury in some tissues. Damage accumulation is therefore proposed to occur via a material fatigue, which is shown to be consistent with observed delays in widespread cavitation activity.

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Shelby B. Hutchens

Papers

In situ Mechanical Testing Reveals Periodic Buckle Nucleation and Propagation in Carbon Nanotube Bundles

Directly Measuring the Complete Stress–Strain Response of Ultrathin Polymer Films

Analysis of uniaxial compression of vertically aligned carbon nanotubes

Elastic cavitation and fracture via injection

Cavitation-induced damage of soft materials by focused ultrasound bursts: A fracture-based bubble dynamics model