Structural features of biobased composite foams revealed by X-ray tomography.

Polymer foams can have heterogeneous and complex internal structures, especially when material blends or particles have been integrated to create composites. It becomes even more challenging to probe and understand foam structure/properties when using non-uniform particles, such as biobased fillers. Optical or SEM imaging can only provide limited information as these are two-dimensional (2D) surface techniques. In this study, 3D X-ray tomography was applied to comprehensively analyze the structural features of biobased polyurethane foams containing porous rice hull fillers. The in-depth characterization at a wide range of length scale enabled us to quantify and obtain statistics of the unique trends in foam pore size and pore orientation corresponding to rice hull particle fraction and particle size. Rice hull particles were found to induce smaller cell formation. In addition, these biobased particles influenced cell expansion and caused cells to have less consistent orientation. Furthermore, after foam samples were subjected to cyclic compressive loading, X-ray tomography showed fractures in large (>100 µm) particles. This helps reveal the premature failing mechanism of composite foams with highly porous and coarse particles. The study elucidates novel microstructural evolution and deformation mechanisms using 3D X-ray tomography. The results offer new insights on internal structures for biobased composites and foams that are not previously possible through the conventional characterization tools.

Cholla cactus wood (Cylindropuntia imbricata): Hierarchical structure and micromechanical properties.

The Cholla cactus is a species of cacti that survives in arid environments and produces a unique mesh-like porous wood. In this article, we present a comprehensive investigation on the hierarchical structure and micromechanical properties of the Cholla cactus wood. Multiple approaches consisting of X-ray tomography, scanning electron microscopy, scanning probe microscopy, nanoindentation, and finite element simulations were used to gain insight into the structure, property, and design principles of the Cholla cactus wood. The microstructure of the Cholla cactus wood consists of different components, including vessels, rays, and fibers. In the present study, we quantitatively describe the structure of each of these wood components and their likely functions, both from the perspective of biological and mechanical behavior. Nanoindentation experiments revealed for the first time that the cell walls of the fibers exhibit stiffness and hardness higher than those of rays. Furthermore, the idea of making porous, thin-walled cylinders was abstracted from the design of vessel elements, and the structures inspired by this principle were studied in tensile and torsional loading conditions using finite element simulations. Finite element simulations revealed that the utilization of a larger volume of material to carry the load leads to an increase in toughness of these structures, and thus suggested that the pores should be architected to maximize the distribution of load. STATEMENT OF SIGNIFICANCE: The Cholla cactus wood possess a unique hierarchical structure that enables it to thrive in arid environments. Our correlative microscopy approach reveals incredible strategies that individual wood components exhibit to enable the survival of Cholla cactus in extreme environments. The present work quantifies the microstructure and mechanical properties of this very interesting natural system. We further investigate a design principle inspired by the vessel elements, one of the wood components of Cholla cactus, using finite element simulations. The study presented here advances our understanding of the structural significance of Cholla cactus and potentially other desert plants and will further help design architected structural materials.

In situ investigations of failure mechanisms of silica fibers from the venus flower basket (Euplectella Aspergillum).

The fibers of the deep-sea sponge Euplectella aspergillum exhibit exceptional mechanical properties due to their unique layered structure at a micrometer length scale. In the present study, we utilize a correlative approach comprising of in situ tensile testing inside a scanning electron microscope (SEM) and post-failure fractography to precisely understand mechanisms through which layered architecture of fibers fracture and improves damage tolerance in tensile loading condition. The real-time observation of fibers in the present study confirms for the first time that the failure starts from the surface of fibers and proceeds to the center through successive layers. The concentric layers surrounding the central core sacrifice themselves and protect the central core through various toughening mechanisms like crack deflection, crack arrest, interface debonding, and fiber pullout. STATEMENT OF SIGNIFICANCE: Biological materials often exhibit multiscale hierarchical structures that can be incorporated into the design of next generation of engineering materials. The fibers of deep-sea sponge E. aspergillum possess core-shell like layered architecture. Our in situ study reveals astounding strategies by which this architecture delays the fracture of the fiber. The core-shell architecture of these fibers behaves like fiber-reinforced ceramic matrix composite, where the outer shells act as a matrix and the central core acts as a fiber. The outer shells take the environmental brunt and scarify themselves to protect the central core. The precise understanding of damage evolution presented here will help to design architected materials for load-bearing applications.

Unraveling the Mechanisms of the Apis mellifera Honeycomb Construction by 4D X-ray Microscopy.

Honeycomb is one of nature's best engineered structures. Even though it has inspired several modern engineering structures, an understanding of the process by which the hexagonal cells are formed in 3D space is lacking. Previous studies on the structure of the honeycomb are based on either 2D microscopy or by direct visual observations. As a result, several critical features of its microstructure and the precise mechanisms of its growth are not well understood. Using 4D X-ray microscopy, this study shows how individual and groups of honeycomb cells are formed. Cells grow additively from a corrugated central spine in a dynamic manner. The previously undocumented, corrugated spine contributes significantly to the comb's robust mechanical properties in all three dimensions. As cells grow, honey bees create a "coping," which this study shows to be the location where new wax material is deposited behind where compaction and densification take place. This is exemplified by pores in the wax observed at the coping and alternating rear junctions between the comb cells that arise from the additive building technique and the highly efficient cell packing methodology, respectively. Additional mechanisms for growth and formation are discussed and described.

The Comparative approach to bio-inspired design: integrating biodiversity and biologists into the design process.

Biodiversity provides a massive library of ideas for bio-inspired design, but the sheer number of species to consider can be daunting. Current approaches for sifting through biodiversity to identify relevant biological models include searching for champion adapters that are particularly adept at solving a particular design challenge. While the champion adapter approach has benefits, it tends to focus on a narrow set of popular models while neglecting the majority of species. An alternative approach to bio-inspired design is the comparative method, which leverages biodiversity by drawing inspiration across a broad range of species. This approach uses methods in phylogenetics to map traits across evolutionary trees and compare trait variation to infer structure-function relationships. Although comparative methods have not been widely used in bio-inspired design, they have led to breakthroughs in studies on gecko-inspired adhesives and multifunctionality of butterfly wing scales. Here we outline how comparative methods can be used to complement existing approaches to bioinspired design, and we provide an example focused on bio-inspired lattices, including honeycomb and glass sponges. We demonstrate how comparative methods can lead to breakthroughs in bio-inspired applications as well as answer major questions in biology, which can strengthen collaborations with biologists and produce deeper insights into biological function.

Reducing the risk of rostral bending failure in Curculio Linnaeus, 1758.

With over 300 species worldwide, the genus Curculio Linnaeus, 1758 is a widespread, morphologically diverse lineage of weevils that mainly parasitize nuts. Females use the rostrum, an elongate cuticular extension of the head, to excavate oviposition sites. This process causes extreme bending and deformation of the rostrum, without apparent harm to the structure. The cuticle of the rostral apex exhibits substantial modifications to its composite structure that enhance the elasticity and resiliency of this structure. Here we develop finite element models of the head and rostrum for three Curculio species representing disparate North American clades and rostral morphotypes. The models were subjected to varying apical loads and to prescribed dislocation of the head capsule, with and without representing the cuticular modifications of the rostral apex. We found that the altered layer thicknesses and macrofiber orientation angles of the rostral apex fully explain the observed elasticity of the rostrum. These modifications have a synergistic effect that greatly enhances the flexibility of the rostral apex. Consequently, the cuticle composite profile of the rostral apex substantially mitigates the risk of fracture in dorso-apical flexion. Removing the cuticular modifications, in turn, causes a negative margin of safety for rostral bending, implying strong risk of catastrophic structural failure. The occipital sulci were identified as an important source of biomechanical constraint upon the elasticity of the rostrum, and exhibit the greatest risk of failure within this structure. The apical cuticle profile greatly reduced the maximum stresses and strain energy accumulated in the rostrum, thereby resulting in a positive margin of safety and reducing the risk of fracture. Our findings imply that the primary selective pressure influencing the evolution of the rostral cuticle was most likely negative selection of structural failure caused by bending. STATEMENT OF SIGNIFICANCE: Weevils are among the most diverse and evolutionarily successful animal lineages on Earth. Their success is driven in part by a structure called the rostrum, which gives weevil heads a characteristic "snout-like" appearance. Nut weevils in the genus Curculio use the rostrum to drill holes into developing fruits and nuts, into which they deposit their eggs. During oviposition this exceedingly slender structure is bent into a straightened configuration - in some species up to 90∘ - but does not suffer any damage during this process. Using finite element models of the rostra of three morphologically distinct species, we show that the Curculio rostrum is only able to withstand repeated, extreme bending because of modifications to the composite structure of the cuticle in the rostral apex. These modifications were shown previously to enhance the intrinsic toughness of the cuticle; in this study, we demonstrate that modification of the rostral cuticle also results in more evenly distributed bending stresses, further reducing the risk of fracture. This is the first time that the laminate profile, orthotropic behavior, and functional gradation of the cuticle have been incorporated into a three-dimensional finite element model of an insect cuticular structure. Our models highlight the significance of biomechanical constraint - i.e., avoidance of catastrophic structural failure - on the evolution of insect morphology.

Bioinspired Honeycomb Core Design: An Experimental Study of the Role of Corner Radius, Coping and Interface.

The honeybee's comb has inspired the design of engineering honeycomb core that primarily abstract the hexagonal cell shape and exploit its mass minimizing properties to construct lightweight panels. This work explored three additional design features that are part of natural honeybee comb but have not been as well studied as design features of interest in honeycomb design: the radius at the corner of each cell, the coping at the top of the cell walls, and the interface between cell arrays. These features were first characterized in natural honeycomb using optical and X-ray techniques and then incorporated into honeycomb core design and fabricated using an additive manufacturing process. The honeycomb cores were then tested in out-of-plane compression and bending, and since all three design features added mass to the overall structure, all metrics of interest were examined per unit mass to assess performance gains despite these additions. The study concluded that the presence of an interface increases specific flexural modulus in bending, with no significant benefit in out-of-plane compression; coping radius positively impacts specific flexural strength, however, the corner radius has no significant effect in bending and actually is slightly detrimental for out-of-plane compression testing.

Ligand Crosslinking Boosts Thermal Transport in Colloidal Nanocrystal Solids.

The ongoing interest in colloidal nanocrystal solids for electronic and photonic devices necessitates that their thermal-transport properties be well understood because heat dissipation frequently limits performance in these devices. Unfortunately, colloidal nanocrystal solids generally possess very low thermal conductivities. This very low thermal conductivity primarily results from the weak van der Waals interaction between the ligands of adjacent nanocrystals. We overcome this thermal-transport bottleneck by crosslinking the ligands to exchange a weak van der Waals interaction with a strong covalent bond. We obtain thermal conductivities of up to 1.7 Wm-1 K-1 that exceed prior reported values by a factor of 4. This improvement is significant because the entire range of prior reported values themselves only span a factor of 4 (i.e., 0.1-0.4 Wm-1 K-1 ). We complement our thermal-conductivity measurements with mechanical nanoindentation measurements that demonstrate ligand crosslinking increases Young's modulus and sound velocity. This increase in sound velocity is a key bridge between mechanical and thermal properties because sound velocity and thermal conductivity are linearly proportional according to kinetic theory. Control experiments with non-crosslinkable ligands, as well as transport modeling, further confirm that ligand crosslinking boosts thermal transport.

Avoidance of Catastrophic Structural Failure as an Evolutionary Constraint: Biomechanics of the Acorn Weevil Rostrum.

The acorn weevil (Curculio Linnaeus, 1758) rostrum (snout) exhibits remarkable flexibility and toughness derived from the microarchitecture of its exoskeleton. Modifications to the composite profile of the rostral cuticle that simultaneously enhance the flexibility and toughness of the distal portion of the snout are characterized. Using classical laminate plate theory, the effect of these modifications on the elastic behavior of the exoskeleton is estimated. It is shown that the tensile behavior of the rostrum across six Curculio species with high morphological variation correlates with changes in the relative layer thicknesses and orientation angles of layers in the exoskeleton. Accordingly, increased endocuticle thickness is strongly correlated with increased tensile strength. Rostrum stiffness is shown to be inversely correlated with work of fracture; thus allowing a highly curved rostrum to completely straighten without structural damage. Finally, exocuticle rich invaginations of the occipital sutures are identified both as a likely site of crack initiation in tensile failure and as a source of morphological constraint on the evolution of the rostrum in Curculio weevils. It is concluded that avoidance of catastrophic structural failure, as initiated in these sutures under tension, is the driving selective pressure in the evolution of the female Curculio rostrum.

Granule formation and structure from single drop impact on heterogeneous powder beds.

Single drop impact of liquid on a static powder bed was studied to investigate the granule formation mechanism, droplet penetration time, as well as the characterization of granules (morphology, surface structure and internal structure). Water was used as the liquid and two pharmaceutical powders, microcrystalline cellulose (MCC) and acetaminophen (APAP), were mixed to make heterogeneous powder beds. The complete drop impact and penetration was recorded by a high speed camera. Two granule formation mechanisms that have been identified previously occurred: Spreading and Tunneling. Spreading occurred for mixtures with an APAP amount of less than 20%, while Tunneling started to occur when the APAP amount increased above 20%. With an increase of APAP concentration, the mean particle size decreased, drop penetration time increased, and the granules formed became smaller in size, which was in good agreement with previous literature. The granule morphology, surface structure, and internal structure were characterized by a prism method with image analysis, scanning electron microscopy (SEM), and X-ray microtomography, respectively. The Spreading mechanism produced flat disks with a porous internal structure, while the Tunneling mechanism produced round granules with a dense internal structure. There is a clear trend of decreasing porosity and increasing roundness of granules made from heterogeneous mixtures within the transition from Spreading to Tunneling. It is believed that the mean particle size of the powder bed and the powder-liquid contact angle are the predominant factors in influencing the formation mechanism, drop penetration time, and granule properties.

Probing Novel Microstructural Evolution Mechanisms in Aluminum Alloys Using 4D Nanoscale Characterization.

Dispersions of nanoscale precipitates in metallic alloys have been known to play a key role in strengthening, by increasing their strain hardenability and providing resistance to deformation. Although these phenomena have been extensively investigated in the last century, the traditional approaches employed in the past have not rendered an authoritative microstructural understanding in such materials. The effect of the precipitates' inherent complex morphology and their 3D spatial distribution on evolution and deformation behavior have often been precluded. This study reports, for the first time, implementation of synchrotron-based hard X-ray nanotomography in Al-Cu alloys to measure kinetics of different nanoscale phases in 3D, and reveals insights behind some of the observed novel phase transformation reactions. The experimental results of the present study reconcile with coarsening models from the Lifshitz-Slyozov-Wagner theory to an unprecedented extent, thereby establishing a new paradigm for thermodynamic analysis of precipitate assemblies. Finally, this study sheds light on the possibilities for establishing new theories for dislocation-particle interactions, based on the limitations of using the Orowan equation in estimating precipitation strengthening.

Accurate stochastic reconstruction of heterogeneous microstructures by limited x-ray tomographic projections.

An accurate knowledge of the complex microstructure of a heterogeneous material is crucial for its performance prediction, prognosis and optimization. X-ray tomography has provided a nondestructive means for microstructure characterization in 3D and 4D (i.e. structural evolution over time), in which a material is typically reconstructed from a large number of tomographic projections using filtered-back-projection (FBP) method or algebraic reconstruction techniques (ART). Here, we present in detail a stochastic optimization procedure that enables one to accurately reconstruct material microstructure from a small number of absorption contrast x-ray tomographic projections. This discrete tomography reconstruction procedure is in contrast to the commonly used FBP and ART, which usually requires thousands of projections for accurate microstructure rendition. The utility of our stochastic procedure is first demonstrated by reconstructing a wide class of two-phase heterogeneous materials including sandstone and hard-particle packing from simulated limited-angle projections in both cone-beam and parallel beam projection geometry. It is then applied to reconstruct tailored Sn-sphere-clay-matrix systems from limited-angle cone-beam data obtained via a lab-scale tomography facility at Arizona State University and parallel-beam synchrotron data obtained at Advanced Photon Source, Argonne National Laboratory. In addition, we examine the information content of tomography data by successively incorporating larger number of projections and quantifying the accuracy of the reconstructions. We show that only a small number of projections (e.g. 20-40, depending on the complexity of the microstructure of interest and desired resolution) are necessary for accurate material reconstructions via our stochastic procedure, which indicates its high efficiency in using limited structural information. The ramifications of the stochastic reconstruction procedure in 4D materials science are also discussed.

Nanoscale Three-Dimensional Microstructural Characterization of an Sn-Rich Solder Alloy Using High-Resolution Transmission X-Ray Microscopy (TXM).

Three-dimensional (3D) nondestructive microstructural characterization was performed using full-field transmission X-ray microscopy on an Sn-rich alloy, at a spatial resolution of 60 nm. This study highlights the use of synchrotron radiation along with Fresnel zone plate optics to perform absorption contrast tomography for analyzing nanoscale features of fine second phase particles distributed in the tin matrix, which are representative of the bulk microstructure. The 3D reconstruction was also used to quantify microstructural details of the analyzed volume.

A multilayer micromechanical model of the cuticle of Curculio longinasus Chittenden, 1927 (Coleoptera: Curculionidae).

Curculio longinasus Chittenden, 1927 (Coleoptera: Curculionidae), is a weevil species common throughout the southwestern United States that uses its rostrum - a very slender, curved, beak-like projection of the head - to excavate tunnels in plant organs (such as acorns) for egg laying (oviposition). Once the apical portion of the rostrum has been inserted into the preferred substrate for oviposition, the female begins rotating around the perimeter of the hole, elevating her head by extending the fore-legs, and rotating the head in place in a drilling motion. This action causes significant elastic deformation of the rostrum, which will bend until it becomes completely straight. To better understand the mechanical behavior of the cuticle as it undergoes deformation during the preparation of oviposition sites, we develop a comprehensive micro/macro model of the micromechanical structure and properties of the cuticle, spanning across all cuticular regions, and reliably mirroring the resultant macroscale properties of the cuticle. Our modeling approach relies on the use of multi-scale, hierarchical biomaterial representation, and employs various micromechanical schemata - e.g., Mori-Tanaka, effective field, and Maxwell - to calculate the homogenized properties of representative volume elements at each level in the hierarchy. We describe the configuration and behavior of this model in detail, and discuss the theoretical implications and limitations of this approach with emphasis on future biomechanical and comparative evolutionary research. Our detailed account of this approach can thereby serve as a methodological template for exploring the biomechanical behavior of new insect structures.

Note: design and construction of a multi-scale, high-resolution, tube-generated x-ray computed-tomography system for three-dimensional (3D) imaging.

The design and construction of a high resolution modular x-ray computed tomography (XCT) system is described. The approach for meeting a specified set of performance goals tailored toward experimental versatility is highlighted. The instrument is unique in its detector and x-ray source configuration, both of which enable elevated optimization of spatial and temporal resolution. The process for component selection is provided. The selected components are specified, the custom component design discussed, and the integration of both into a fully functional XCT instrument is outlined. The novelty of this design is a new lab-scale detector and imaging optimization through x-ray source and detector modularity.