Publications

For an up-to-date list of publications, please visit Google Scholar.

2024

Controlling splat boundary network evolution towards the development of strong and ductile cold sprayed refractory metals: The role of powder characteristics

Mahsa Amiri, Kliah N. Soto Leytan, Diran Apelian, Daniel R. Mumm, Lorenzo Valdevit, Materials Science & Engineering A 902 (2024) 146559

Abstract

Feedstock powder characteristics such as composition (specific alloying elements and concentrations and impurity levels), microstructure, thickness/composition of surface oxide layers, and particle size distribution play a crucial role in determining the overall mechanical properties of cold sprayed deposits. Herein, we report on two deposits consolidated via cold spray processing from differently-sourced batches of nominally identical elemental refractory powders under identical spraying conditions, which exhibit bending strength and ductility values that differ by more than a factor of two – and with the weakest sample displaying negligible effective ductility. Through chemical, microstructural and micromechanical characterization of both the feedstock powders and cold sprayed deposits, we consider the possible influences of feedstock characteristics on the mechanical performance of cold spray consolidated deposits. It is shown that while differences in interstitial oxygen and hydrogen content may result in differences in the intrinsic yield characteristics of the feedstock material, both feedstocks maintain the ductile behavior required to induce good metallurgical bonding upon impact of optimally sized powder particles. We conclude that the deposits formed from the two feedstock powders are indistinguishable and exhibit high ductility when characterized locally within the relatively undeformed bulk of a single particle or splat. However, the two sprayed deposits show low ductility or brittle behavior when loaded in tension across intersplat boundary domains comprising material that has undergone extensive deformation. In addition, one feedstock incorporates a broader particle size distribution, with a long tail of larger-than-optimal particles. These larger particles are accelerated below the critical impact velocity, resulting in observed imperfect metallurgical bonding at splat interfaces and higher porosity at such intersplat boundaries. This result, combined with the overall differences in the morphology of the intersplat boundary network between the two deposits, explains the difference in macroscopic mechanical behavior. We conclude that accurate control of the powder feedstock particle size distribution is essential for optimizing the mechanical integrity of cold sprayed refractory elements and alloys. 

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Microstructural Control of a Multi-Phase PH Steel Printed with Laser Powder Bed Fusion

Brandon Fields, Mahsa Amiri, Jungyun Lim, Julia T. Pürstl, Matthew R. Begley, Diran Apelian, and Lorenzo Valdevit, Adv. Mater. Technol. 2024, 9, 2301037

Abstract

The established approach to materials design for additive manufacturing (AM) consists of attempting to reproduce the uniform structures and properties of conventionally processed materials. While this certainly helped facilitate material certification and the rapid introduction of AM technologies in several industries, the opportunity to exploit unique features of specific AM processes to generate spatially varying microstructures–and hence novel materials, remains largely untapped. This work presents a method for manufacturing materials through laser powder bed fusion (LPBF), in which control over the spatial variation in phase composition and mechanical properties is achieved. This technique is demonstrated using 17-4 precipitation-hardened stainless steel (17-4PH), by controlling spatial modulation of energy densities during printing. This results in local control of ferrite/martensite volume fractions, allowing the fabrication of metal/metal architected composites with hard/brittle regions interspersed with soft/tough regions. Local variations of ˜20% in tensile strength and ˜150% in elongation are achieved, with a spatial resolution of ˜100 microns. The approach is general and robust, fully compatible with commercially available LPBF equipment, and applicable to virtually any multi-phase alloy system. This work shifts the paradigm from attempting to print components with uniform properties to manufacturing alloys with controlled spatial property gradients.

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Investigation of an additively manufactured modified aluminum 7068 alloy: Processing, microstructure, and mechanical properties

Brandon Fields, Mahsa Amiri, Benjamin E. MacDonald, Julia T. Pürstl, Chen Dai, Xiaochun Li, Diran Apelian, Lorenzo Valdevit, Materials Science & Engineering A 891 (2024) 145901

Abstract

Many additively manufactured alloys exhibit higher strengths than compositionally identical alloys processed via conventional processing routes. However, this enhancement is not consistently observed in 7xxx series aluminum alloys. These alloys present two complications when printed via Laser Powder Bed Fusion (LPBF): significant evaporation of strengthening elements from the melt pool and hot cracking during solidification. To address these issues, we introduce two modifications to the feedstock powder: (i) we increase the concentration of alloying constituents to counteract evaporation during printing, and (ii) we disperse TiC nanoparticles within the feedstock powder to promote heterogeneous nucleation and limit grain growth, thus avoiding hot cracking and improving strength. Relationships between the evaporation of alloying elements and laser energy density are quantified experimentally using inductively-coupled-plasma mass-spectrometry and are well captured by simple analytical models. The microstructures in as-printed and heat-treated conditions are characterized using X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Printing parameters have been optimized to attain minimum porosity, resulting in tensile strengths up to 650 MPa, which are in good agreement with predictions from classic models of strengthening mechanisms. 

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Towards a self-healing aluminum metal matrix composite: Design, fabrication, and demonstration

David Svetlizky, Baolong Zheng, Xin Wang, Sen Jiang, Lorenzo Valdevit, Julie M. Schoenung, Enrique J. Lavernia, Noam Eliaz, Applied Materials Today 37 (2024) 102148

Abstract

This paper presents a novel approach to designing and synthesizing a self-healing aluminum-based metal matrix composite (MMC) at the macro-scale. The composite comprises an Al 5083 matrix embedded with low melting point particles (LMPPs) that act as healing agents. A two-step electroless micro-encapsulation process is developed to create LMMPs with a diffusion and thermal barrier designed to protect the Zn-8Al core with a Co-P shell. The MMC is fabricated using spark plasma sintering. Following controlled total fracture under tension, external compressive force is applied during heat treatment to heal the fracture effectively. The evolution of phases and interfaces is characterized using electron microscopy, and transient liquid phase bonding (TLPB) is identified as the fracture-healing mechanism, facilitated in areas with sufficiently high Zn concentration to fill the crack. The design can be expanded to incorporate other matrix and LMMP materials, mechanical crack volume reduction by integrating shape memory alloy (SMA) reinforcement during MMC synthesis, and processing of the self-healing MMC using Directed Energy Deposition additive manufacturing. 

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A multi-scale process for mechanical characterization of ceramic materials produced by Direct Ink Writing

Raphael Thiraux, Alexander D. Dupuy, Kate M. Ainger, Lorenzo Valdevit, Open Ceramics 17 (2024) 100544

Abstract

Mechanical characterization of ceramics is challenging, as the statistical nature of their strength requires numerous specimens to extract reliable distribution parameters. Here, we first propose a high-throughput testing procedure that allows extraction of statistical information on the strength of ceramic materials. We process large numbers of bending specimens from low volumes of material via Direct Ink Writing (DIW), and rapidly characterize them to extract Weibull parameters for bending strength. After investigating five ceramics and downselecting two formulations, we develop a multi-scale procedure to explore the impact of printing-induced defects on the strength distribution of DIW-processed ceramics. Finally, we demonstrate that a judicious choice of the printing strategy produces porous architected structures which can significantly exceed the strength of fully dense DIW-produced monolithic materials. While the results are presented on DIW-processed alumina-based ceramics, the approach is versatile and can provide rapid statistical data on the strength of many ceramic materials. 

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Neural network for predicting Peierls barrier spectrum and its influence on dislocation motion

Xinyi Wang, Lorenzo Valdevit, Penghui Cao, Acta Materialia 267 (2024) 119696

Abstract

The Peierls barrier represents the inherent lattice resistance to dislocation glide, controlling dislocation movement and dictating the resulting mechanical properties. The rise of multi-principal element alloys, with their vast compositional space and local chemical fluctuations, introduces notable challenges in efficiently computing the Peierls barriers. Here, we propose a neural network model that captures the chemistry and structure of screw dislocations. By incorporating two crucial inputs, the local atomic type and displacement, our model enables accurate and efficient prediction of the Peierls barriers in multi-component space. Using this neural network, we construct a barrier diagram across the entire ternary space of refractory Nb-Mo-Ta alloys, from which the compositions with high or low barriers can be quickly identified. We discover that the NbMo binary alloy can have a higher barrier than NbMoTa ternary system, suggesting chemical complexity may not be the predominant factor governing dislocation barrier. Subsequently, three screened compositions with different barriers are selected for studying their effects on dislocation motion. Atomistic simulations reveal that a higher mean barrier slows down dislocation mobility, while a broader distribution of barriers facilitates kink pair nucleation, altering the rate-limiting process from kink pair nucleation to kink glide and cross kinking. This study presents a general neural network model that enables rapid screening composition with the desired barrier spectrum and will impact the exploration and discovery of alloys with improved dislocation-controlled properties. 

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The defect sensitivity of brittle truss-based metamaterials
Patrick Ziemke, Owen Finney, Ryan G. Chambers, Raphael Thiraux, Lorenzo Valdevit, Matthew R. Begley, Materials & Design 239 (2024) 112776
Abstract
Architected strut-based metamaterials fabricated via three-dimensional printing exhibit a wide range of geometric and material heterogeneity, including variations in strut size, surface roughness, embedded micro-cracks and disconnected struts. The locations and severity of these defects are highly variable; combined with the complexity of the structure itself, it is exceedingly difficult to identify critical defects that limit performance and inform qualification protocols. To address this challenge, we consider the impact of distributions of defects for various strut-based lattice topologies. The role of defects is analyzed using Weibull distributions of strut failure strains. We relate the statistical distributions of strut properties to macroscopic stress-strain performance, using high through-put finite element predictions in thousands of virtual tests. Increasing the prevalence of defects decreases macroscopic strength; however, this has the complementary effect of introducing apparent ductility, i.e. load capacity even after the onset of strut failures. Hence, there is a trade-off between achieving high strength and gradual loss of stiffness that is desirable for thermal loading or lattice cores. Predictions of average strength as a function of Weibull modulus provide knock-down factors relative to the defect-free strength. In turn, these clearly identify quantitative processing targets to mitigate the impact of defects.
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2023

In situ observation of melt pool evolution in ultrasonic vibration‑assisted directed energy deposition

Salma A. El‑Azab, Cheng Zhang, Sen Jiang, Aleksandra L. Vyatskikh, Lorenzo Valdevit, Enrique J. Lavernia, Julie M. Schoenung, Scientific Reports (2023) 13:17705

Abstract

The presence of defects, such as pores, in materials processed using additive manufacturing represents a challenge during the manufacturing of many engineering components. Recently, ultrasonic vibration-assisted (UV-A) directed energy deposition (DED) has been shown to reduce porosity, promote grain refinement, and enhance mechanical performance in metal components. Whereas it is evident that the formation of such microstructural features is affected by the melt pool behavior, the specific mechanisms by which ultrasonic vibration (UV) influences the melt pool remain elusive. In the present investigation, UV was applied in situ to DED of 316L stainless steel single tracks and bulk parts. For the first time, high-speed video imaging and thermal imaging were implemented in situ to quantitatively correlate the application of UV to melt pool evolution in DED. Extensive imaging data were coupled with in-depth microstructural characterization to develop a statistically robust dataset describing the observed phenomena. Our findings show that UV increases the melt pool peak temperature and dimensions, while improving the wettability of injected particles with the melt pool surface and reducing particle residence time. Near the substrate, we observe that UV results in a 92% decrease in porosity, and a 54% decrease in dendritic arm spacing. The effect of UV on the melt pool is caused by the combined mechanisms of acoustic cavitation, ultrasound absorption, and acoustic streaming. Through in situ imaging we demonstrate quantitatively that these phenomena, acting simultaneously, effectively diminish with increasing build height and size due to acoustic attenuation, consequently decreasing the positive effect of implementing UV-A DED. Thus, this research provides valuable insight into the value of in situ imaging, as well as the effects of UV on DED melt pool dynamics, the stochastic interactions between the melt pool and incoming powder particles, and the limitations of build geometry on the UV-A DED technique.

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Residual stress mitigation in directed energy deposition

Aleksandra L. Vyatskikh, Xin Wang, James Haley, Baolong Zheng, Lorenzo Valdevit, Enrique J. Lavernia, Julie M. Schoenung, Materials Science & Engineering A 871 (2023) 144845

Abstract

Directed Energy Deposition (DED), a class of additive manufacturing techniques, has seen rapid growth over the last decade for potential applications in aerospace, medical devices, and energy systems. Despite notable progress in the research and development of AM, control and mitigation of residual stress during DED remains a challenge. In this work, we propose a novel approach that can be used for the mitigation of residual stresses in additively manufactured components. Specifically, we propose to mitigate the residual stress state of as-deposited components using alloy design, engineering of solid-state transformations, and the introduction of both hard and soft metallic phases. We demonstrate this strategy with a model system consisting of pure Fe and Fe–Cu. Experimental results indicate that residual stresses can be successfully manipulated by adjusting the alloy composition as a soft metallic phase can accommodate plastic deformation. Moreover, our findings suggest that the solid-state transformations experienced by the Fe and Fe-rich phases contribute to the observed differences in magnitude and location of residual stresses. This study is the first to suggest using residual stress as an engineering criterion in the design of alloys for metal additive manufacturing. 

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Influence of co-deposition strategy on the mechanical behavior of additively manufactured functionally integrated materials

Benjamin E. MacDonald , Baolong Zheng , Brandon Fields, Xin Wang , Sen Jiang , Penghui Cao , Lorenzo Valdevit , Enrique J. Lavernia , Julie M. Schoenung, Additive Manufacturing 61 (2023) 103328

Abstract

The co-deposition of multiple powder feedstocks during metal additive manufacturing (AM) can be used to fabricate materials with spatially dependent properties, which can be engineered to contain different function- alities (i.e., functionally integrated materials, FIMs). Although the transition region that forms between dissimilar materials has been studied in detail, the influence of co-deposition on the resultant spatial phase distribution and associated mechanical behavior has heretofore not been reported. In this study, FIM samples transitioning from stainless steel (SS) 316 L to Haynes 282 Ni-based superalloy were deposited via directed energy deposition (DED). The FIM samples were compared to baseline, homogeneous single-alloy deposited samples using digital image correlation during tensile testing, together with microscopy, energy-dispersive X-ray spectroscopy, elec- tron backscattered diffraction, and thermodynamic modeling, to assess the performance of different co- deposition strategies. Each FIM sample exhibited a compositionally and microstructurally unique transition re- gion from SS 316 L to Haynes 282, which was found to have implications on the strain localization across the transition region during uniaxial tensile loading. Finer step sizes in co-deposition were found to minimize strain localization by avoiding sharp compositional interfaces in the transition region.

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Design, material, function, and fabrication of metamaterials

Amir A. Zadpoor, Mohammad J. Mirzaali, Lorenzo Valdevit, and Jonathan B. Hopkins, APL Mater. 11, 020401 (2023)

Abstract

Metamaterials are engineered materials with unusual, unique properties and advanced functionalities that are a direct consequence of their microarchitecture. While initial properties and functionalities were limited to optics and electromagnetism, many novel categories of metamaterials that have applications in many different areas of research and practice, including acoustic, mechanics, biomaterials, and thermal engineering, have appeared in the last decade. This editorial serves as a prelude to the special issue with the same title that presents a number of selected studies in these directions. In particular, we review some of the most important developments in the design and fabrication of metamaterials with an emphasis on the more recent categories. We also suggest some directions for future research.

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Deformation behavior of cell walls in an additively manufactured hybrid metallic foam
Xin Wang, Baolong Zheng, Hangman Chen, Dongxu Liu, Kehang Yu, Benjamin E. MacDonald, Lorenzo Valdevit, Lizhi Sun, Penghui Cao, Enrique J. Lavernia, Julie M. Schoenung, Additive Manufacturing 61 (2023) 103365
Abstract
A hybrid Al-Al3Ni metallic foam was synthesized in-situ via directed energy deposition (DED) of Ni-coated Al 6061 powder, without the need for a foaming agent. Three-dimensional characterization via X-ray computed tomography shows that the foam contains approximately 61.5 % porosity and a high volume fraction of the Al3Ni phase (~60 vol. %) within the cell walls. This microstructure is notably distinct from the eutectic structure that is typically observed in conventionally processed Al-Ni alloys. To investigate the mechanical properties and deformation mechanisms of the Al-Al3Ni cell walls, in-situ micro-pillar compression was performed, and the results reveal a notable yield strength of 560 MPa and a compressive strain that exceeds 30 %. These properties are attributable to the presence of a high volume fraction of Al3Ni particles, in combination with the charac- teristics of the Al/Al3Ni interfaces. To provide insight into the deformation mechanisms in the cell walls we used in-situ mechanical testing, transmission electron microscopy and precession electron diffraction characterization, together with molecular dynamics simulations. Our results reveal two distinct mechanisms: uniform dislocation- based deformation of the Al alloy phase and localized deformation within the slip bands in the Al3Ni phase. The results further highlight the importance of the Al/Al3Ni interfaces in mechanical strengthening and the transfer of plastic deformation from the Al phase to the Al3Ni phase. At high mechanical loads, cracks form due to the large stress concentration at the slip bands and slip band intersections in the Al3Ni, giving rise to intragranular fracture of Al3Ni and finally interfacial debonding and cracking.
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2022

Nanoarchitected metal/ceramic interpenetrating phase composites
Jens Bauer, Martí Sala-Casanovas, Mahsa Amiri, Lorenzo Valdevit, Science Advances 8 (2022) eabo3080
Abstract

Architected metals and ceramics with nanoscale cellular designs, e.g., nanolattices, are currently subject of extensive investigation. By harnessing extreme material size effects, nanolattices demonstrated classically inaccessible properties at low density, with exceptional potential for superior lightweight materials. This study expands the concept of nanoarchitecture to dense metal/ceramic composites, presenting co-continuous architectures of three- dimensional printed pyrolytic carbon shell reinforcements and electrodeposited nickel matrices. We demonstrate ductile compressive deformability with elongated ultrahigh strength plateaus, resulting in an extremely high combination of compressive strength and strain energy absorption. Simultaneously, property-to-weight ratios outperform those of lightweight nanolattices. Superior to cellular nanoarchitectures, interpenetrating nanocom- posites may combine multiple size-dependent characteristics, whether mechanical or functional, which are radically antagonistic in existing materials. This provides a pathway toward previously unobtainable multifunctionality, extending far beyond lightweight structure applications.

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Minimal Surface-Based Materials for Topological Elastic Wave Guiding
Yuning Guo, Matheus Inguaggiato Nora Rosa, Mohit Gupta, Benjamin Emerson Dolan, Brandon Fields, Lorenzo Valdevit, and Massimo Ruzzene, Adv. Funct. Mater. (2022) 2204122

Abstract

Materials based on minimal surface geometries have shown superior strength and stiffness at low densities, which makes them promising continuous-based material platforms for a variety of engineering applications. In this work, it is demonstrated how these mechanical properties can be complemented by dynamic functionalities resulting from robust topological guiding of elastic waves at interfaces that are incorporated into the consid- ered material platforms. Starting from the definition of Schwarz P minimal surface, geometric parametrizations are introduced that break spatial sym- metry by forming 1D dimerized and 2D hexagonal minimal surface-based materials. Breaking of spatial symmetries produces topologically non-trivial interfaces that support the localization of vibrational modes and the robust propagation of elastic waves along pre-defined paths. These dynamic prop- erties are predicted through numerical simulations and are illustrated by performing vibration and wave propagation experiments on additively manu- factured samples. The introduction of symmetry-breaking topological inter- faces through parametrizations that modify the geometry of periodic minimal surfaces suggests a new strategy to supplement the load-bearing properties of this class of materials with novel dynamic functionalities.

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Damage tolerance in additively manufactured ceramic architected materials
Raphael Thiraux, Alexander D. Dupuy, Tianjiao Lei, Timothy J. Rupert, Ali Mohraz, Lorenzo Valdevit, Journal of the European Ceramic Society 42 (2022) 5893-5903

Abstract

Technical ceramics exhibit exceptional high-temperature properties, but unfortunately their extreme crack sensitivity and high melting point make it challenging to manufacture geometrically complex structures with sufficient strength and toughness. Emerging additive manufacturing technologies enable the fabrication of large- scale complex-shape artifacts with architected internal topology; when such topology can be arranged at the microscale, the defect population can be controlled, thus improving the strength of the material. Here, ceramic micro-architected materials are fabricated using direct ink writing (DIW) of an alumina nanoparticle-loaded ink, followed by sintering. After characterizing the rheology of the ink and extracting optimal processing parameters, the microstructure of the sintered structures is investigated to assess composition, density, grain size and defect population. Mechanical experiments reveal that woodpile architected materials with relative densities of 0.38–0.73 exhibit higher strength and damage tolerance than fully dense ceramics printed under identical conditions, an intriguing feature that can be attributed to topological toughening.

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Alleviating expansion-induced mechanical degradation in lithium-ion battery silicon anodes via morphological design
Sierra J. Gross, Meng-Ting Hsieh, Daniel R. Mumm, Lorenzo Valdevit, Ali Mohraz, Extreme Mechanics Letters 54 (2022) 101746

Abstract

The mechanics of films undergoing volume expansion on curved substrates plays a key role in a variety of technologies including biomedical implants, thermal and environmental barrier coatings, and electrochemical energy storage systems. Silicon anodes for lithium-ion batteries are an especially challenging case because they can undergo volume variations up to 300% that results in cracking, delamination, and thus significant loss in performance. In this study, we use finite element analysis to model the volume expansion during lithiation for silicon coated on spinodal, inverse opal, gyroid, and Schwartz primitive nickel backbones and compare the distributions of maximum principal stress, strain energy density, and von Mises stress, which we use as indicators for propensity for cracking, delamination, and yielding, in order to explore the effect of backbone morphology on mechanical degradation during expansion. We show that, when compared to the inverse opal, the spinodal morphology reduces and uniformly distributes the maximum principal stress and strain energy density in the silicon layer, and delays the onset of expansion-induced yielding at all silicon layer thicknesses, which we ascribe to the unique interfacial curvature distribution of spinodal structures. This work highlights the importance of morphology on coatings undergoing volume variations and unveils the particular promise of spinodally derived materials for the design of next generation lithium-ion battery electrodes.

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2021

Thickness-Dependent Microstructure in Additively Manufactured Stainless Steel
Alexandra L. Vyatskikh, Thomas B. Slagle, Sen Jiang, Salma A. El-Azab, Umberto Scipioni Bertoli, Lorenzo Valdevit, Enrique J. Lavernia, and Julie M. Schoenung, Journal of Materials Engineering and Performance 30 (2021) 6606-6617

Abstract

Widespread industrial adoption of metal additive manufacturing (AM) requires an in-depth understanding of microstructural evolution during AM. In this study, the effect of process parameters and feature thickness on the microstructures of 316L stainless steel components fabricated by laser powder bed fusion (LPBF) was examined. A standard benchmark geometry developed by the National Institute of Standards and Technology, which contained walls of 0.5, 2.5 and 5.0 mm in thickness, was used. Optical microscopy, finite element analysis, scanning electron microscopy and electron backscatter diffraction revealed dramatic microstructural differences in features of different thickness within the same component. The feature thickness influenced the cooling rate, which in turn impacted the melt pool size, solidification microstructure, grain morphology and density of geometrically necessary dislocations. The relationship between feature size and grain morphology was dependent on the energy input used during LPBF. Such behavior suggested that local manipulation of LPBF process parameters can be employed to achieve microstructural homogeneity within the as-printed stainless steel components.

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Tensegrity Metamaterials: Toward Failure-Resistant Engineering Systems through Delocalized Deformation
Jens Bauer, Julie A. Kraus, Cameron Crook, Julian J. Rimoli, Lorenzo Valdevit, Advanced Materials 33 (2021) 2005647

Abstract

Failure of materials and structures is inherently linked to localized mechanisms, from shear banding in metals, to crack propagation in ceramics and collapse of space-trusses after buckling of individual struts. In lightweight structures, localized deformation causes catastrophic failure, limiting their application to small strain regimes. To ensure robustness under real-world nonlinear loading scenarios, overdesigned linear-elastic constructions are adopted. Here, the concept of delocalized deformation as a pathway to failure-resistant structures and materials is introduced. Space-tileable tensegrity metamaterials achieving delocalized deformation via the discontinuity of their compression members are presented. Unprecedented failure resistance is shown, with up to 25-fold enhancement in deformability and orders of magnitude increased energy absorption capability without failure over same-strength state-of-the-art lattice architectures. This study provides important groundwork for design of superior engineering systems, from reusable impact protection systems to adaptive load-bearing structures.

A press release on this article is available here.

A link to a video emphasizing the main concept of this work can be found here.

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Nanoscale investigation of two-photon polymerized microstructures with tip-enhanced Raman spectroscopy
Anastasiya V Kazantseva, Elena A Chernykh, Cameron Crook, Evan P Garcia, Dmitry A Fishman, Eric O Potma, Lorenzo Valdevit, Sergey S Kharintsev, Tommaso Baldacchini, J Phys Photonics 3 (2021) 024001

Abstract

We demonstrate the use of tip-enhanced Raman spectroscopy (TERS) on polymeric microstructures fabricated by two-photon polymerization direct laser writing (TPP-DLW). Compared to the signal intensity obtained in confocal Raman microscopy, a linear enhancement of almost two times is measured when using TERS. Because the probing volume is much smaller in TERS than in confocal Raman microscopy, the effective signal enhancement is estimated to be ca. 10^4. We obtain chemical maps of TPP microstructures using TERS with relatively short acquisition times and with high spatial resolution as defined by the metallic tip apex radius of curvature. We take advantage of this high resolution to study the homogeneity of the polymer network in TPP microstructures printed in an acrylic-based resin. We find that the polymer degree of conversion varies by about 30% within a distance of only 100 nm. The combination of high resolution topographical and chemical data delivered by TERS provides an effective analytical tool for studying TPP-DLW materials in a non-destructive way.

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Mechanically Compliant Thermal Interfaces Using Biporous Copper-Polydimethylsiloxane Interpenetrating Phase Composite
Cheng-Hui Lin, Anna Guell Izard, Lorenzo Valdevit, Yoonjin Won, Advanced Materials Interfaces 8 (2021) 2001423

Abstract

Thermal interface materials are essential for thermal management in electronics packaging by providing a low resistance thermal pathway between heat sources and heat sinks. Nanostructured materials can be potential candidates for the next-generation interface materials by coupling their high thermal conductivity and mechanical compliance, suppressing failure even after large numbers of thermal cycles. This work investigates the thermal and mechanical characteristics of a new type of thermal interface materials, consisting of metal/elastomer interpenetrating phase composites. The 3D, highly porous copper scaffolds are fabricated via a fast and simple in situ bubble-templated electrodeposition process without the presence of solid templates; subsequently, the void fraction of the composite is filled by elastomer infiltration. The presence of elastomer matrix demonstrates limited impact on the thermal conductivity of the composite while it contributes substantially to the mechanical properties, providing the structural flexibility required. Thermal resistance values of 1.2–4.0 cm^2 K W^-1 are measured upon multiple thermal cycles, confirming the mechanical stability of the composite, without showing any noticeable degradation.

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Mechanical performance of 3D printed interpenetrating phase composites with spinodal topologies
Yunfei Zhang, Meng-Ting Hsieh, Lorenzo Valdevit, Composite Structures 263 (2021) 113693

Abstract

The mechanical response of interpenetrating phase composites (IPCs) with stochastic spinodal topologies is investigated experimentally and numerically. Model polymeric systems are fabricated by Polyjet multi‐material printing, with the reinforcing phase taking the topology of a spinodal shell, and the remaining volume filled by a softer matrix. We show that spinodal shell IPCs have comparable compressive strength and stiffness to IPCs with two well‐established periodic reinforcements, the Schwarz P triply periodic minimal surface (TPMS) and the octet truss‐lattice, while exhibiting far less catastrophic failure and greater damage resistance, particularly at high volume fraction of reinforcing phase. The combination of high stiffness and strength and a long flat plateau after yielding makes spinodal shell IPCs a promising candidate for energy absorption and impact protection applications, where the lack of material softening upon large compressive strains can prevent sudden collapse. Importantly, in contrast with all IPCs with periodic reinforcements, spinodal shell IPCs are amenable to scalable manufacturing via self‐assembly techniques.

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Architected implant designs for long bones: Advantages of minimal surface-based topologies
Meng-Ting Hsieh, Matther R. Begley, Lorenzo Valdevit, Materials & Design 207 (2021) 109838

Abstract

Large bone fractures often require porous implants for complete healing. In this work, we numerically investigate the suitability of three topologically very different architected materials for long bone implants: the octet truss-based lattice, the Schwartz P minimal surface-based lattice and the spinodal stochastic surface-based lattice. Each implant topology (reinforcement) and its surrounding tissue (soft matrix) are modeled as a composite system via finite element analysis. Performance metrics are defined based on the Young’s modulus, the peak stress under service conditions, the interfacial surface area per unit volume and the relative bone growth rate (estimated based on the strain transferred to the soft matrix). We show that surface-based topologies are less prone to fatigue failure and may promote supe- rior bone growth than conventional truss-based designs. Spinodal surface-based architected materials have the best performance, and can be fabricated via self-assembly approaches followed by material con- version, potentially allowing scalable fabrication of implants with unit cell sizes at the micro-scale, thus dramatically amplifying surface area per unit volume and bone growth efficiency.

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2020

Thermal post-curing as an efficient strategy to eliminate process parameter sensitivity in the mechanical properties of two-photon polymerized materials
Jens Bauer, Anna Guell Izard, Yunfei Zhang, Tommaso Baldacchini, Lorenzo Valdevit, Opt Express, 2020 vol. 28 (14) pp. 20362-20371

Abstract

Two-photon polymerization direct laser writing (TPP-DLW) is one of the most versatile technologies to additively manufacture complex parts with nanoscale resolution. However, the wide range of mechanical properties that results from the chosen combination of multiple process parameters imposes an obstacle to its widespread use. Here we introduce a thermal post-curing route as an effective and simple method to increase the mechanical properties of acrylate-based TPP-DLW-derived parts by 20-250% and to largely eliminate the characteristic coupling of processing parameters, material properties and part functionality. We identify the underlying mechanism of the property enhancement as a self-initiated thermal curing reaction, which robustly facilitates the high property reproducibility that is essential for any application of TPP-DLW.

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Surface oxide and hydroxide effects on aluminum microparticle impact bonding
Jasper Lienhard, Cameron Crook, Maryam Zahiri Azar, Mostafa Hassani, Daniel R. Mumm, David Veysset, Diran Apelian, Keith A. Nelson, Victor Champagne, Aaron Nardi, Christopher A. Schuh, Lorenzo Valdevit
Acta Materialia, 197 (2020) 28-39
Abstract

Oxides, hydroxides, and other surface films act as impediments to metallurgical bonding during cold spray impact adhesion, raising the critical adhesion velocity and reducing the quality of the deposited coating. Using a single-particle impact imaging approach we study how altering the passivating surface oxides with exposures to various levels of heat and humidity affect the cold spray critical adhesion veloc- ity in the case of aluminum. We analyze the thickness, composition and microstructure of the passivation layers with transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and Fourier- transform infrared spectroscopy (FTIR), and correlate our observations with a direct measurement of the critical adhesion velocity for each surface treatment. We conclude that exposures to temperatures as high as 300 °C for up to 240 min in dry air, or to room-temperature with humidity levels as high as 50% for 4 days, have negligible effect on the surface oxide layers, and by extension do not affect the critical adhesion velocity. In contrast, ambient-temperature exposure to 95% relative humidity levels for 4 days increases the critical adhesion velocity by more than 125 m/s, approximately a 14% percent increase. We observe that this distinct change in critical adhesion velocity is correlated with unique changes in the passivating layer thickness, thickness uniformity, crystallinity and composition resulting from exposure to high humidity. These results speak to particle surface treatments to improve the cold spray process.

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Plate-nanolattices at the theoretical limit of stiffness and strength
Cameron Crook, Jens Bauer, Anna Guell Izard, Cristine Santos de Oliveira, Juliana Martins de Souza e Silva, Jonathan B. Berger, Lorenzo Valdevit
Nature Communications, 1–11. http://doi.org/10.1038/s41467-020-15434-2
Abstract
Though beam-based lattices have dominated mechanical metamaterials for the past two decades, low structural efficiency limits their performance to fractions of the Hashin-Shtrikman and Suquet upper bounds, i.e. the theoretical stiffness and strength limits of any isotropic cellular topology, respectively. While plate-based designs are predicted to reach the upper bounds, experimental verification has remained elusive due to significant manufacturing challenges. Here, we present a new class of nanolattices, constructed from closed-cell plate-architectures. Carbon plate-nanolattices are fabricated via two-photon lithography and pyrolysis and shown to reach the Hashin-Shtrikman and Suquet upper bounds, via in situ mechanical compression, nano-computed tomography and micro-Raman spectroscopy. Demonstrating specific strengths surpassing those of bulk diamond and average performance improvements up to 639% over the best beam-nanolattices, this study provides detailed experimental evidence of plate architectures as a superior mechanical metamaterial topology.
See an exciting Seeker video on this work: https://youtu.be/0KJjs4W09hQ
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Minisurf – A minimal surface generator for finite element modeling and additive manufacturing
Meng-Ting Hsieh, Lorenzo Valdevit
Software Impacts 6 (2020) 100026
Abstract
Triply periodic minimal surfaces (TPMSs) have long been studied by mathematicians but have recently garnered significant interest from the engineering community as ideal topologies for shell-based architected materials with both mechanical and functional applications. Here, we present a TPMS generator, MiniSurf. It combines surface visualization and CAD file generation (for both finite element modeling and additive manufacturing) within one single GUI. MiniSurf presently can generate 19 built-in and one user-defined triply periodic minimal surfaces based on their level-set surface approximations. Users can fully control the periodicity and precision of the generated surfaces. We show that MiniSurf can potentially be a very useful tool in designing and fabricating architected materials.
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Enhanced adhesion in two-photon polymerization direct laser writing
A. Guell Izard, E. P. Garcia, M. Dixon, E. O. Potma, T. Baldacchini, L. Valdevit
AIP Advances, 10, 045217
Abstract
We have quantified the adhesion forces between two-photon polymerization direct laser writing (TPP-DLW) microstructures and glass surfaces with and without an adhesion promoter. Glass surfaces treated with an acryloxy-silane agent produce adhesion forces that are almost three times larger than the forces observed with pristine glass surfaces. Determination of the substrates’ surface free energies suggests that the observed adhesion enhancement is chemical in its nature, implying that covalent bonds are formed between the polymer and the glass by means of the silane agent. The importance of this finding is demonstrated in the successful production of glassy carbon microstructures using TPP-DLW, followed by pyrolysis.
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A versatile numerical approach for calculating the fracture toughness and R-curves of cellular materials
Meng-Ting Hsieh, Vikram S. Deshpande, Lorenzo Valdevit
Journal of the Mechanics and Physics of Solids, 138, 103925–18
Abstract
We develop a numerical methodology for the calculation of mode-I R-curves of brittle and elastoplastic lattice materials, and unveil the impact of lattice topology, relative density and constituent material behavior on the toughening response of 2D isotropic lattices. The approach is based on finite element calculations of the J-integral on a single-edge-notch- bend (SENB) specimen, with individual bars modeled as beams having a linear elastic or a power-law elasto-plastic constitutive behavior and a maximum strain-based damage model. Results for three 2D isotropic lattice topologies (triangular, hexagonal and kagome) and two constituent materials (representative of a brittle ceramic (silicon carbide) and a strain hardening elasto-plastic metal (titanium alloy)) are presented. We extract initial frac- ture toughness and R-curves for all lattices and show that (i) elastic brittle triangular lat- tices exhibit toughening (rising R-curve), and (ii) elasto-plastic triangular lattices display significant toughening, while elasto-plastic hexagonal lattices fail in a brittle manner. We show that the difference in such failure behavior can be explained by the size of the plastic zone that grows upon crack propagation, and conclude that the nature of crack propaga- tion in lattices (brittle vs ductile) depends both on the constituent material and the lattice architecture. While results are presented for 2D truss-lattices, the proposed approach can be easily applied to 3D truss and shell-lattices, as long as the crack tip lies within the empty space of a unit cell.
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2019

Ultrahigh Energy Absorption Multifunctional Spinodal Nanoarchitectures
A. Guell Izard, J. Bauer, C. Crook, V. Turlo, L. Valdevit
Small (2019) 1903834
Abstract

Nanolattices are promoted as next-generation multifunctional high-performance materials, but their mechanical response is limited to extreme strength yet brittleness, or extreme deformability but low strength and stiffness. Ideal impact protection systems require high-stress plateaus over long deformation ranges to maximize energy absorption. Here glassy carbon nanospinodals, i.e., nanoarchitectures with spinodal shell topology, combining ultrahigh energy absorption and exceptional strength and stiffness at low weight. Noncatastrophic deformation up to 80% strain, and energy absorption up to one order of magnitude higher than for other nano-, micro-, macro-architectures and solids, and state-of-the-art impact protection structures are shown. At the same time, the strength and stiffness are on par with the most advanced yet brittle nanolattices, demonstrating true multifunctionality. Finite element simulations show that optimized shell thickness-to-curvature-radius ratios suppress catastrophic failure by impeding propagation of dangerously oriented cracks. In contrast to most micro- and nano-architected materials, spinodal architectures may be easily manufacturable on an industrial scale, and may become the next generation of superior cellular materials for structural applications.

 

This article was reviewed in Science by Senior Editor Marc Lavine.

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Thermal transport in hollow metallic microlattices
S. Farzinazar, T. A. Schaedler, L. Valdevit, J. Lee
APL Materials 7 (2019) 101108
Abstract
While over the past decade architected cellular materials have been shown to possess unique mechanical properties, their thermal properties have received relatively little attention. Here, we investigate thermal transport in hollow nickel microlattices as a function of temperature and mechanical loading using infrared thermography. The effective thermal conductivity of hollow nickel microlattices with 99.9% porosity and 1 µm layer thickness is as low as 0.049 W m−1 K−1 at 320 K and increases to 0.075 W m−1 K−1 at 480 K, an increase we attribute to internal thermal radiation. By measuring the emissivity and using the Stephan-Boltzmann law, we estimate the contribution of thermal radiation in the effective thermal conductivity to range from 20% at 320 K to 49% at 480 K. The high porosity of microlattices strongly limits solid conduction and makes surface radiation very important in thermal transport. We further explore the impact of the strut surface condition by comparing hollow doped nickel microlattices with a smooth surface to those with a rough surface: the emissivity increases from 0.24 to 0.43, leading to increased thermal radiation contributions of 41% at 320 K to 58% at 480 K. Under mechanical loading, as the strain increases from 0% to 50%, decreasing the angle between the struts and the horizontal plane from 60° to 38°, the effective thermal conductivity decreases from 0.049 W m−1 K−1 to 0.016 W m−1 K−1. These findings indicate that architected cellular materials provide an excellent platform to control thermal properties independently on mechanical properties and to potentially develop thermal and thermomechanical metamaterials.
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The mechanical response of cellular materials with spinodal topologies
M-T. Hsieh, B. Endo, Y. Zhang, J. Bauer, L. Valdevit
Journal of the Mechanics and Physics of Solids 125 (2019) 401-419
Abstract
The mechanical response of cellular materials with spinodal topologies is numerically and experimentally investigated. Spinodal microstructures are generated by the numerical solution of the Cahn-Hilliard equation. Two different topologies are investigated: ‘solid models,’ where one of the two phases is modeled as a solid material and the remaining volume is void space; and ‘shell models,’ where the interface between the two phases is assumed to be a solid shell, with the rest of the volume modeled as void space. In both cases, a wide range of relative densities and spinodal characteristic feature sizes are investigated. The topology and morphology of all the numerically generated models are carefully characterized to extract key geometrical features and ensure that the distribution of curvatures and the aging law are consistent with the physics of spinodal decomposition. Finite element meshes are generated for each model, and the uniaxial compressive stiffness and strength are extracted. We show that while solid spinodal models in the density range of 30-70% are relatively inefficient (i.e., their strength and stiffness exhibit a high-power scaling with relative density), shell spinodal models in the density range of 0.01-1% are exceptionally stiff and strong. Spinodal shell materials are also shown to be remarkably imperfection insensitive. These findings are verified experimentally by in-situ uniaxial compression of polymeric samples printed at the microscale by Direct Laser Writing (DLW). At low relative densities, the strength and stiffness of shell spinodal models outperform those of most lattice materials and approach theoretical bounds for isotropic cellular materials. Most importantly, these materials can be produced by self-assembly techniques over a range of length scales, providing unique scalability.
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Scalable synthesis of gyroid-inspired freestanding three-dimensional graphene architectures
A. E. Garcia, C. Santillan Wang, R. N. Sanderson, K. M. McDevitt, Y. Zhang, L. Valdevit, D. R. Mumm, A. Mohraz, R. Ragan
Nanoscale Adv. 1 (2019) 3870-3882
Abstract
Three-dimensional porous architectures of graphene are desirable for energy storage, catalysis, and sensing applications. Yet it has proven challenging to devise scalable methods capable of producing co-continuous architectures and well-defined, uniform pore and ligament sizes at length scales relevant to applications. This is further complicated by processing temperatures necessary for high quality graphene. Here, bicontinuous interfacially jammed emulsion gels (bijels) are formed and processed into sacrificial porous Ni scaffolds for chemical vapor deposition to produce freestanding three-dimensional turbostratic graphene (bi-3DG) monoliths with high specific surface area. Scanning electron microscopy (SEM) images show that the bi-3DG monoliths inherit the unique microstructural characteristics of their bijel parents. Processing of the Ni templates strongly influences the resultant bi-3DG structures, enabling the formation of stacked graphene flakes or fewer-layer continuous films. Despite the multilayer nature, Raman spectra exhibit no discernable defect peak and large relative intensity for the Raman 2D mode, which is a characteristic of turbostratic graphene. Moiré patterns, observed in scanning tunneling microscopy images, further confirm the presence of turbostratic graphene. Nanoindentation of macroscopic pillars reveals a Young’s modulus of 30 MPa, one of the highest recorded for sp2 carbon in a porous structure. Overall, this work highlights the utility of a scalable self-assembly method towards porous high quality graphene constructs with tunable, uniform, and co-continuous microstructure.
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Programmable Mechanical Properties of Two-Photon Polymerized Materials: From Nanowires to Bulk
J. Bauer, A. Guell Izard, Y. Zhang, T. Baldacchini, L. Valdevit
Advanced Materials Technologies 4 (2019) 1900146
Abstract
Two-photon polymerization direct laser writing (TPP-DLW) is the most promising technology for additive manufacturing of geometrically complex parts with nanoscale features, and could dramatically accelerate the development of a wide range of engineering micro/nanosystems. However, a major obstacle to TPP-DLW’s widespread industrial adoption is the lack of systematic data on material properties and limited knowledge on their correlation with processing parameters. These correlations for the acrylate-based resin IP-Dip are experimentally established over a large range of process parameters and length scales ranging from nanometers to centimeters. Universal characteristic relations between mechanical properties and process parameters are identified, which enable the tailoring of the material strength and stiffness over half an order of magnitude from rubbery soft to hard and strong. With a threshold-based optics model presented herein, the mechanical properties of the two-photon polymerized material can be accurately captured as a function of the applied process parameters, laying the foundation for a universal quantitative predictability of two-photon polymerization with programmable mechanical properties. This knowledge enables fabrication of microscale components with tailored local gradients in their mechanical properties, with significant implications for the development of novel mechanical, photonic, and photonic metamaterials.
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Negative-Stiffness Inclusions as a Platform for Real-Time Tunable Phononic Metamaterials
L. Salari-Sharif, B. Haghpanah, A. Guell Izard, M. Tootkaboni, L. Valdevit
Physical Review Applied 11 (2019) 024062
Abstract
We propose an approach for real-time manipulation of low-frequency phononic band gaps in a metamaterial without affecting the material geometry, microarchitecture, or the crystal structure of the base material. Metamaterials with tunable band gaps are realized by introducing periodically arranged negative-stiffness inclusions, the modulus of which can be varied in time in order to modify the metamaterial macroscopic stiffness in certain directions without bringing the material to the point of elastic instability or inducing extreme geometric change. The evolution of band gaps is investigated numerically, and the proposed concept is verified experimentally in a lattice prototype with magnetic elements functioning as negative-stiffness units. Design guidelines for achieving a real-time tunable phononic band gap are also presented.
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Multiscale modeling and optimization of the mechanics of hierarchical metamaterialsoes Here
D. M. Kochmann, J. B. Hopkins, L. Valdevit
MRS Bulletin 44 (2019) 773-781
Abstract

We present a survey of modeling techniques used to describe and predict architected cellular metamaterials, and to optimize their topology and geometry toward tailoring their mechanical properties such as stiffness, strength, fracture toughness, and energy absorption. Architectures of interest include truss-, plate-, and shell-based networks with and without periodicity, whose effective mechanical behavior is simulated by tools such as classical finite elements, further scale-bridging techniques such as homogenization and concurrent scale-coupling, and effective continuum descriptions of the underlying discrete networks. In addition to summarizing advances in applying the latter techniques to improve the properties of metamaterials and featuring prominent examples of structure–property relations achieved this way, we also present recently introduced techniques to improve the optimization process toward a full exploitation of the available design space, accounting for both linear and nonlinear material behavior.

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Magnetoelastic Metamaterials for Energy Dissipation and Wave Filtering
A. Guell Izard, L. Valdevit
Advanced Engineering Materials (2019) 1901019-7
Abstract

A novel magnetoelastic mechanical metamaterial consisting of a hyperelastic 2D lattice incorporating permanent magnets is presented and characterized. When properly designed and fabricated, the metamaterial possesses two stable equilibrium configurations (henceforth referred to as hexagonal/hourglass and kagome), both stretching dominated (and hence stiff ). The two configurations have significantly different elastic properties and wave propagation characteristics, as shown numerically and experimentally. By switching between the two configurations via uniaxial loading cycles, the material displays hysteresis, thus dissipating substantial amounts of energy; in contrast with purely mechanical bistable structures (e.g., arches, hinged beams and buckled beams), the proposed magnetoelastic metamaterial does not require multiple unit cells in series or stiff boundary conditions to exhibit energy dissipation, thus enabling the implementation of compact stiff dampers. The presence of a bandgap in the kagome configuration (but not in the hexagonal/hourglass configuration) is attributed to an internal resonance mechanism and provides the foundation for the development of compact dynamic filters for mechanical signals.

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Additive Manufacturing of Ductile, Ultrastrong Polymer-Derived Nanoceramics
J. Bauer, C. Crook, A. Guell Izard, Z. C. Eckel, N. Ruvalcaba, T. A. Schaedler, L. Valdevit
Matter (2019)
Abstract

Ceramics would be ideal engineering materials if their brittleness and scattered fracture strength could be overcome. While ductility and extraordinary strength have been reported at the nanoscale, they both rapidly disappear when samples reach micrometer dimensions; furthermore, manufacturing is limited to elaborate approaches, which are purely scientific in nature. Here, we present a robust route to additively manufacture ductile, ultrastrong silicon oxycarbide (SiOC) via two-photon polymerization direct laser writing (TPP-DLW) of a preceramic resin and subsequent pyrolysis. We 3D-print micrometer-size pillars and architected materials with feature sizes down to ∼200 nm and characterize them under uniaxial compression. Independent of size, SiOC micropillars consistently deform plastically with strains up to 25% and strengths >7 GPa, across the entire range of examined diameters (1–20 μm). Our findings demonstrate straightforward fabrication of ductile, ultrastrong ceramics at previously unprecedented scales, potentially enabling manufacturing of engineering systems up to tens of millimeters in size.

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2018

The effect of manufacturing defects on compressive strength of ultralight hollow microlattices: A data-driven study
L. Salari-Sharif, S.W. Godfrey, M. Tootkaboni, L. Valdevit
Additive Manufacturing 19 (2018) 51-61
Abstract
Hollow microlattices constitute a model topology for architected materials, as they combine excellent specific stiffness and strength with relative ease of manufacturing. The most scalable manufacturing technique to date encompasses fabrication of a sacrificial polymeric template by the Self Propagating Photopolymer Waveguide (SPPW) process, followed by thin film coating and removal of the substrate. Accurate modeling of mechanical properties (e.g., stiffness, strength) of hollow microlattices is challenging, primarily due to the complex stress state around the hollow nodes and the existence of manufacturing-induced geometric imperfections (e.g. cracks, non-circularity, etc.). In this work, we use a variety of measuring techniques (SEM imaging, CT scanning, etc.) to characterize the geometric imperfections in a nickel-based ultralight hollow microlattice and investigate their effect on the compressive strength of the lattice. At the strut level, where a more quantitative description of geometric defects is available, the gathered data is used to build a stochastic field model of geometric imperfections using Proper Orthogonal Decomposition. Using Monte Carlo simulations, the critical buckling loads of a large set of imperfect bars created using the stochastic model are then extracted by Finite Elements Analysis. The statistics of the buckling strength in artificially generated bars is then used to explain the scatter in the strength of CT-derived bars and its correlation with the lattice strength measured experimentally. Although the quantitative results are specific to microlattices fabricated by SPPW templating, the methodology presented herein is equally applicable to architected materials produced by other manufacturing processes.
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Hybrid Hollow Microlattices with Unique Combinations of Stiffness and Damping
L. Salari-Shrif, T. A. Schaedler, L. Valdevit
ASME Journal of Engineering Materials and Technology 140 (2018) 031003-11
Abstract
Hybrid micro-architected materials with unique combinations of high stiffness, high damping, and low density are presented. We demonstrate a scalable manufacturing pro- cess to fabricate hollow microlattices with a sandwich wall architecture comprising an elastomeric core and metallic skins. In this configuration, the metallic skins provide stiff- ness and strength, whereas the elastomeric core provides constrained-layer damping. This damping mechanism is effective under any strain amplitude, and at any relative den- sity, in stark contrast with the structural damping mechanism exhibited by ultralight metallic or ceramic architected materials, which requires large strain and densities lower than a fraction of a percent. We present an analytical model for stiffness and constrained-layer damping of hybrid hollow microlattices, and verify it with finite ele- ments simulations and experimental measurements. Subsequently, this model is adopted in optimal design studies to identify hybrid microlattice geometries which provide ideal combinations of high stiffness and damping and low density. Finally, a previously derived analytical model for structural damping of ultralight metallic microlattices is extended to hybrid lattices and used to show that ultralight hybrid designs are more efficient than purely metallic ones.
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Damping of selectively bonded 3D woven lattice materials
L. Salari-Sharif, S. M. Ryan, M. Pelacci, J. K. Guest, L. Valdevit, S. Szyniszewski
Scientific Reports 8 (2018) 14572
Abstract
The objective of this paper is to unveil a novel damping mechanism exhibited by 3D woven lattice materials (3DW), with emphasis on response to high-frequency excitations. Conventional bulk damping materials, such as rubber, exhibit relatively low stiffness, while stiff metals and ceramics typically have negligible damping. Here we demonstrate that high damping and structural stiffness can be simultaneously achieved in 3D woven lattice materials by brazing only select lattice joints, resulting in a load-bearing lattice frame intertwined with free, ‘floating’ lattice members to generate damping. The produced material samples are comparable to polymers in terms of damping coefficient, but are porous and have much higher maximum use temperature. We shed light on a novel damping mechanism enabled by an interplay between the forcing frequency imposed onto a load-bearing lattice frame and the motion of the embedded, free-moving lattice members. This novel class of damping metamaterials has potential use in a broad range of weight sensitive applications that require vibration attenuation at high frequencies.
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ARCHITECTED MATERIALS: SYNTHESIS, CHARACTERIZATION, MODELING, AND OPTIMAL DESIGN
Lorenzo Valdevit, Katia Bertoldi, James Guest, Christopher Spadaccini
Journal of Materials Research 33 (2018) 241-246
Abstract

Architected materials are multi-phase and/or cellular materials in which the topological distribution of the phases is carefully controlled and optimized for specific functions or properties. Nearly two decades of research has resulted in the identification of a number of topologically simple, easy to fabricate, well established structures (including honeycombs and truss lattices), which have been optimized for specific stiffness and strength, impact and blast protection, sound absorption, wave dispersion, active cooling and combinations thereof.

Over the past few years, dramatic advances in processing techniques, including polymer-based templating (e.g., stereolithography, photopolymer waveguide prototyping, two-photon polymerization) and direct single- or multi-material formation (e.g., direct laser sintering, deformed metal lattices, 3D weaving and knitting), have enabled fabrication of new architected materials with complex geometry and remarkably precise control over the geometric arrangement of solid phases and voids from the nanometer to the centimeter scale.

The ordered, topologically complex nature of these materials and the degree of precision with which their features can now be defined suggests the development of new multi-physics and multi-scale modeling tools that can enable optimal designs. The result is efficient multi-scale cellular materials with unprecedented ranges of density, stiffness, strength, energy absorption, permeability, chemical reactivity, wave/matter interaction and other multifunctional properties, which promise dramatic advances across important technology areas such as lightweight structures, functional coatings, bio-scaffolds, catalyst supports, photonic/phononic systems and other applications.

Some of the most exciting recent developments in this field are the exploration of size effects in the development of nano-architected materials with superior combinations of properties, the investigation of geometrically complex unit cell architectures that enable non-linear effective mechanical response from linear-elastic materials, novel manufacturing approaches with increased resolution and scalability, and improved design optimization tools. Here we briefly review some recent progress in these areas, and conclude with some thoughts about opportunities for future development. The collection of articles in this focus issue is a wonderful exposure to some of the latest original work in this field.

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2017

Topology optimization of multiphase architected materials for energy dissipation
A. Asadpoure, M. Tootkaboni, L. Valdevit
Computer Methods in Applied Mechanics and Engineering 325 (2017) 314-329
Abstract

In this article, we study the computational design of multiphase architected materials comprising a stiff phase, a dissipative phase, and void space, with enhanced vibration damping characteristics under wave propagation. We develop a topology optimization framework that maximizes a figure of merit comprising of effective stiffness, density and effective damping. We also propose novel material interpolation strategies to avoid the blending of different phases at any given point in the design domain. This is achieved by carefully defining different penalization schemes for different components of the merit function. The effective stiffness of the periodic multiphase material is calculated using homogenization theory and the Bloch–Floquet theorem is used to obtain its damping capacity, allowing for the investigation of the effect of wave directionality, material microarchitecture and intrinsic material properties on the wave attenuation characteristics. It is shown that the proposed topology optimization framework allows for systematic tailoring of microstructure of the multiphase materials for wide ranges of frequencies and densities and results in the identification of optimized multiphase cellular designs with void space that are superior to fully dense topologies.

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Some Graphical Interpretations of Melan's Theorem for Shakedown Design
Vermaak N., Boissier M., Valdevit L., McMeeking R.M.
In: Barrera O., Cocks A., Ponter A. (eds) Advances in Direct Methods for Materials and Structures. Springer (2017)
Abstract
Bree Interaction Diagrams have long been one of the major visual design guides for employing and evaluating shakedown in engineering applications. These diagrams provide representations of the realms in which elastoplastic behaviors, including shakedown, are found for a material and structure under variable loads. The creation of these diagrams often relies upon some combination of upper or lower bound shakedown theorems and numerical shakedown limit determination techniques. Part of the utility of these diagrams is that, for a given structure and loading conditions, inspecting them is sufficient to determine whether shakedown will occur or not. The diagrams cannot however, give the designer insight into how the conditions for shakedown are met. This chapter presents some graphical interpretations of one of the common methods for shakedown determination: the use of Melan’s Lower Bound Theorem. The intent is to provide additional insight for designers regarding how shakedown conditions are satisfied. In this way, additional directions for modifying designs to recover shakedown behavior may also be identified. Revisiting this well-established theorem from a graphical and pedagogical approach, also provides a foundation for interdisciplinary innovation. The particular focus is on simple examples that highlight ways in which Melan’s theorem may be applied to shakedown design problems.
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Optimal design of a cellular material encompassing negative stiffness elements for unique combinations of stiffness and elastic hysteresis
A. Guell, G. McKnight, L. Valdevit
Materials and Design 135 (2017) 37-50
Abstract
Viscoelastic materials are commonly used to dissipate kinetic energy in case of impact and vibrations. Unfortunately, dissipating large amounts of energy in a monolithic material requires high combinations of two intrinsic properties – Young’s modulus and loss factor, which are generally in conflict. This limitation can be overcome by designing cellular materials incorporating negative stiffness elements. Here we investigate a configuration comprising two positive stiffness elements and one negative stiffness element. This unit cell possesses an internal degree of freedom, which introduces hysteresis under a loading-unloading cycle, resulting in substantial energy dissipation, while maintaining stiffness. We demonstrate and optimize a simple implementation in a single material design that does not require external stabilization or pre-compression of buckled elements; these key features make it amenable to fabrication by virtually any additive manufacturing approach (from 3D printing to assembly and brazing) in a wide range of base materials (from polymers to metals). No additional intrinsic damping mechanism is required for the base material, which is assumed linear elastic. Furthermore, the architected material can be designed to be fully recoverable. When optimized, these architected materials exhibit extremely high combinations of Young’s modulus and damping, far superior to those of each constituent phase.
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Nanolattices: An Emerging Class of Mechanical Metamaterials
J. Bauer, L. R. Meza, T. A. Schaedler, R. Schwaiger, X. Zheng, L. Valdevit
Advanced Materials (2017) 1701850 (26p)
Abstract
In 1903, Alexander Graham Bell developed a design principle to generate lightweight, mechanically robust lattice structures based on triangular cells; this has since found broad application in lightweight design. Over one hundred years later, the same principle is being used in the fabrication of nanolattice materials, namely lattice structures composed of nanoscale constituents. Taking advantage of the size-dependent properties typical of nanoparticles, nanowires, and thin films, nanolattices redefine the limits of the accessible material-property space throughout different disciplines. Herein, the exceptional mechanical performance of nanolattices, including their ultrahigh strength, damage tolerance, and stiffness, are reviewed, and their potential for multifunctional applications beyond mechanics is examined. The efficient integration of architecture and size-affected properties is key to further develop nanolattices. The introduction of a hierarchical architecture is an effective tool in enhancing mechanical properties, and the eventual goal of nanolattice design may be to replicate the intricate hierarchies and functionalities observed in biological materials. Additive manufacturing and self-assembly techniques enable lattice design at the nanoscale; the scaling-up of nanolattice fabrication is currently the major challenge to their widespread use in technological applications.
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Elastic Architected Materials with Extreme Damping Capacity
B. Haghpanah, A. Shirazi, L. Salari-Sharif, A. Guell, L. Valdevit
Extreme Mechanics Letters 17 (2017) 56-61
Abstract
We report on a new class of elastic architected materials with hybrid unit cells, consisting of discrete elastic elements with non-convex strain energy and one convex (but possibly nonlinear) elastic element, to obtain a reversible multifunctional material with extreme energy dissipation. The proposed design exploits numerically optimized nonlinearities in the force–displacement response of the sub-unit-cell elements to approach the theoretical limit of specific damping capacity in any material, Psi_th=8. Specific damping capacities up to  Psi=6.02 were experimentally demonstrated, which are far greater than any experimental value previously reported, including in high damping elastomers (Psi<4.5). Remarkably, this damping performance is achieved even with a single unit cell, thus avoiding the need for thick multi-cell designs. Furthermore, the proposed design offers relatively high stiffness and low transmitted stress upon compression. The proposed concept could enable the design of reversible impact-resistant structures with superior crashworthiness and energy dissipation.
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2016

Multistable Shape-Reconfigurable Architected Materials
B. Haghpanah, L. Salari-Sharif, P. Pourrajab, J. Hopkins, L. Valdevit
Advanced Materials 28 (2016) 7915-7920
Abstract

Multistable shape-reconfigurable architected materials encompassing living hinges and enabling combinations of high strength, high volumetric change, and complex shape-morphing patterns are introduced. Analytical and numerical investigations, validated by experiments, are performed to characterize the mechanical behavior of the proposed materials. The proposed architected materials can be constructed from virtually any base material, at any length scale and dimensionality.

This article was featured in a Nature Research Highlight, Nature 535 (07/2016) 32

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A Tri-Leaflet Nitinol Mesh Scaffold for Engineering Heart Valves
SH Alavi, MS Baliarda, N. Bonessio, L. Valdevit, A. Kheradvar
Annals of Biomedical Engineering 45 (2016) 413-426
Abstract
The epidemiology of valvular heart disease has significantly changed in the past few decades with aging as one of the main contributing factors. The available options for replacement of diseased valves are currently limited to mechanical and bioprosthetic valves, while the tissue engineered ones that are under study are currently far from clinical approval. The main problem with the tissue engineered heart valves is their progressive deterioration that leads to regurgitation and/or leaflet thickening a few months after implantation. The use of bioresorbable scaffolds is speculated to be one factor affecting these valves’ failure. We have previously developed a non-degradable superelastic nitinol mesh scaffold concept that can be used for heart valve tissue engineering applications. It is hypothesized that the use of a non-degradable superelastic nitinol mesh may increase the durability of tissue engineered heart valves, avoid their shrinkage, and accordingly prevent regurgitation. The current work aims to study the effects of the design features on mechanical characteristics of this valve scaffold to attain proper function prior to in vivo implantation.
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2015

Topology optimization of lightweight periodic lattices under simultaneous compressive and shear stiffness constraints
A. Asadpoure, L. Valdevit
International Journal of Solids and Structures 60-61 (2015) 1-16
Abstract
This paper investigates the optimal architecture of planar micro lattice materials for minimum weight under simultaneous axial and shear stiffness constraints. A well-established structural topology opti- mization approach is used, where the unit cell is composed of a network of beam elements (Timoshenko beams are used instead of truss elements to allow modeling of bending-dominated architectures); start- ing from a dense unit cell initial mesh, the algorithm progressively eliminates inefficient elements and resizes the essential load-bearing elements, finally converging to an optimal unit cell architecture. This architecture is repeated in both directions to generate the infinite lattice. Hollow circular cross-sections are assumed for all elements, although the shape of the cross-section has minimal effect on most optimal topologies under the linear elasticity assumption made throughout this work. As optimal designs identi- fied by structural topology optimization algorithms are strongly dependent on initial conditions, a careful analysis of the effect of mesh connectivity, unit cell aspect ratio and mesh density is conducted. This study identifies hierarchical lattices that are significantly more efficient than any isotropic lattice (includ- ing the widely studied triangular, hexagonal and Kagomé lattices) for a wide range of axial and shear stiff- ness combinations. As isotropy is not always a design requirement (particularly in the context of sandwich core design, where shear stiffness is generally more important than compressive stiffness), the- se optimal architectures can outperform any established topology. Extension to 3D lattices is straightforward.
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Push-to-pull tensile testing of ultra-strong nanoscale ceramic-polymer composites made by additive manufacturing
J. Bauer, A. Schroer, R. Schwaiger, I. Tesari, C. Lange, L. Valdevit, O. Kraft
Extreme Mechanics Letters 3 (2015) 105-112
Abstract
The search for light yet strong materials recently benefited from novel high resolution 3D-printing technologies, which allow for fabricating lightweight porous materials with optimally designed micro-topologies. Architectural design improves mechanical properties significantly compared to stochastic porosity, as in foams. Miniaturization of the architectures offers to exploit material strengthening size-effects occurring at the nanoscale. However, these effects and their interaction with structural behavior are not yet well understood. We present tensile experiments of nanoscale alumina–polymer composite bars and cellular microarchitectures, applying 3D-printed push-to-pull mechanisms. The strength of alumina is found to strongly increase as the material thickness decreases. Below 50 nm thickness a plateau at about 5.5 GPa is reached, which is in the range of the theoretical strength. The characteristic low tensile strength of ceramics and its high variability seem not to hold at the nanoscale. Thus, when designed and fabricated appropriately, microarchitectures will facilitate carrying these size-effects beyond scales in future, allowing the use of ceramic materials far beyond what is possible to date.
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Novel insights from 3D models: the pivotal role of physical symmetry in epithelial organization
A. Kurup, T. Tran, M. Keating, P. Gascard, L. Valdevit, T. Tlsty, E. Botvinick
Scientific Reports 5 (2015) 15153
Abstract
3D tissue culture models are utilized to study breast cancer and other pathologies because they better capture the complexity of in vivo tissue architecture compared to 2D models. However, to mimic the in vivoenvironment, the mechanics and geometry of the ECM must also be considered. Here, we studied the mechanical environment created in two 3D models, the overlay protocol (OP) and embedded protocol (EP). Mammary epithelial acini features were compared using OP or EP under conditions known to alter acinus organization, i.e. collagen crosslinking and/or ErbB2 receptor activation. Finite element analysis and active microrheology demonstrated that OP creates a physically asymmetric environment with non-uniform mechanical stresses in radial and circumferential directions. Further contrasting with EP, acini in OP displayed cooperation between ErbB2 signalling and matrix crosslinking. These differences in acini phenotype observed between OP and EP highlight the functional impact of physical symmetry in 3D tissue culture models.
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Macroscopic strain controlled ion current in an elastomeric microchannel
C-C. Kuo, Y. Li, D. Nguyen, S. Buchsbaum, L. Innes, A. P. Esser-Kahn, L. Valdevit, L. Sun, Z. Siwy, M. Dennin
Journal of Applied Physics 117 (2015) 174904
Abstract
We report on the fabrication of an ultra-high aspect ratio ionically conductivesingle microchannel with tunable diameter from ≈ 20 μm to fully closed. The 4 mm-long channel is fabricated in a Polydimethylsiloxane (PDMS) mold and its cross-sectional area is controlled by applying macroscopic compressive strain to the mold in a direction perpendicular to the channel length. We investigated the ionic conduction properties of the channel. For a wide range of compressive strain up to ≈ 0.27, the strain dependence of the resistance is monotonic and fully reversible. For strain > 0.27, ionic conduction suddenly shuts off and the system becomes hysteretic (whereby a finite strain reduction is required to reopen the channel). Upon unloading, the original behavior is retrieved. This reversible behavior is observed over 200 compression cycles. The cross-sectional area of the channel can be inferred from the ion current measurement,as confirmed by a Nano-Computed Tomography investigation. We show that the cross-sectional area decreases monotonically with the applied compressive strain in the reversible range, in qualitative agreement with linear elasticity theory. We find that the shut-off strain is affected by the spatial extent of the applied strain, which provides additional tunability. Our tunable channel is well-suited for multiple applications in micro/nano-fluidic devices.
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Incorporating Fabrication Cost into Topology Optimization of Discrete Structures and Lattices
A. Asadpoure, J. Guest, L. Valdevit
Structural and Multidisciplinary Optimization 51 (2015) 385-396
Abstract
In this article, we propose a method to incorporate fabrication cost in the topology optimization of light and stiff truss structures and periodic lattices. The fabrication cost of a design is estimated by assigning a unit cost to each truss element, meant to approximate the cost of element placement and associated connections. A regularized Heaviside step function is utilized to estimate the number of elements existing in the design domain. This makes the cost function smooth and differentiable, thus enabling the application of gradient-based optimization schemes. We demonstrate the proposed method with classic examples in structural engineering and in the design of a material lattice, illustrating the effect of the fabrication unit cost on the optimal topologies. We also show that the proposed method can be efficiently used to impose an upper bound on the allowed number of elements in the optimal design of a truss system. Importantly, compared to traditional approaches in structural topology optimization, the proposed algorithm reduces the computational time and reduces the dependency on the threshold used for element removal.
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2014

Glass-Blown Pyrex Resonator with Compensating Ti Coating for Reduction of TCF
J. Giner de Haro, L. Valdevit, A. Shkel
International Symposium of inertial Sensors and Systems, Laguna Beach, CA, Feb 25, 2014
Abstract
This paper demonstrates that the Thermal Coefficient of resonant Frequency (TCF) of a micro glass-blown Pyrex spherical resonator can be substantially reduced by the application of a titanium (Ti) coating. Finite Elements Analysis (FEA) is used to demonstrate that the temperature dependence of the Young’s modulus of the shell material is the dominant parameter affecting the TCF of the resonator, clearly suggesting the use of a metallic compensating layer. Experimental characterization demonstrates that the TCF of a Pyrex glass-blown resonator is reduced by 70% (from 73 ppm/°C to 24 ppm/°C) by the application of a 1.33 μm thick layer of Ti. It is predicted by FEM that for a Ti layer thickness on the order of 2.5 μm the TCF will fall below 10 ppm an acceptable value for high performance resonators. This investigation is a step forward in the quest to employ the desirable properties of micro-blown resonators, such as high symmetry, manufacturing tolerances and environmental robustness.
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Fabrication and Deformation of Metallic Glass Micro-Lattices
J. Rys, L. Valdevit, T.A. Schaedler, A.J. Jacobsen, W.B. Carter, J.R. Greer
Advanced Engineering Materials 16 (2014) 889-896
Abstract
Recent progress in micro- and nanofabrication techniques enables the creation of hierarchically architected microlattices with dimensional control over six orders of magnitude, from centimeters down to nanometers. This hierarchical control facilitates the exploration of opportunities to exploit nano-sized material effects in structural materials. In this work, we present the fabrication, characterization, and properties of hollow metallic glass NiP microlattices. The wall thicknesses, deposited by electroless plating, were varied from %60 nm up to 600 nm, resulting in relative densities spanning from 0.02 to 0.2%. Uniaxial quasi-static compression tests revealed two different regimes in deformation: (i) Structures with a wall thickness above 150 nm failed by catastrophic failure at the nodes and fracture events at the struts, with significant micro- cracking and (ii) Lattices whose wall thickness was below 150 nm failed initially via buckling followed by significant plastic deformation rather than by post-elastic catastrophic fracture. This departure in deformation mechanism from brittle to deformable exhibited by the thin-walled structures is discussed in the framework of brittle-to-ductile transition emergent in nano-sized metallic glasses.
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Energy Dissipation Mechanisms in Hollow Metallic Microlattices
L. Salari-Sharif, T. A. Schaedler, L. Valdevit
Journal of Materials Research 29 (2014) 1755-1770
Abstract
When properly designed at ultra-low density, hollow metallic microlattices can fully recover from compressive strains in excess of 50%, while dissipating a considerable portion of the elastic strain energy. This article investigates the physical mechanisms responsible for energy loss upon compressive cycling, and attributes the most significant contribution to a unique form of structural damping, whereby elastic local buckling of individual bars releases energy upon loading. Subsequently, a simple mechanical model is presented to capture the relationship between lattice geometry and structural damping. The model is used to optimize the microlattice geometry for maximum damping performance. The conclusions show that hollow metallic microlattices exhibit exceptionally large values of the damping figure of merit, (Young’s modulus)^(1/3) (loss coefficient)/(density), but this performance requires very low relative densities (<1%), thus limiting the amount of energy that can be dissipated.
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Accurate Stiffness Measurement of Ultralight Hollow Metallic Microlattices by Laser Vibrometry
L. Salari-Sharif, L. Valdevit
Experimental Mechanics, 54 (2014) 1491-1495
Abstract
Recent progress in advanced manufacturing enables fabrication of macro-scale hollow metallic lattices with unit cells in the millimeter range and sub-unit cell features at the submicron scale. If designed to minimize mass, these metallic microlattices can be manufactured with densities lower than 1 mg/cm3, making them the lightest metallic materials ever demonstrated. Measuring the compressive stiffness of these ultralight lattices with conventional contact techniques presents a major challenge, as the lattices buckle or locally fracture immediately after contact with the loading platens is established, with associated reduction in stiffness. Non-contact resonant approaches have been successfully used in the past for modulus measurements in solid materials, at both small and large scales. In this work we demonstrate that Laser Doppler Vibrometry coupled with Finite Elements Analysis is a suitable technique for the reliable extraction of the Young’s modulus in ultralight microlattices.
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2013

The Effects of Tine Coupling and Geometrical Imperfections on the Response of DETF Resonators
K. Azgin, L.Valdevit
Journal of Micromechanics and Microengineering, 23 (2013) 125011 (12p)
Abstract
This paper presents a two-degree-of-freedom analytical model for the electromechanical response of double ended tuning fork (DETF) force sensors. The model describes the mechanical interaction between the tines and allows investigation of the effect of a number of asymmetries, in tine stiffness, mass, electromechanical parameters and load sharing between the tines. These asymmetries are introduced during fabrication (e.g., as a result of undercut) and are impossible to completely eliminate in a practical design. The mechanical coupling between the tines induces a frequency separation between the in-phase and the out-of-phase resonant modes. The magnitude of this separation and the relative intensity of the two modes are affected by all the asymmetries mentioned above. Two key conclusions emerge: (i) as the external axial compressive load is increased, the in-phase mode reaches zero frequency (buckling) much faster than the out-of-phase (i.e., operational) mode, resulting in a device with a decreased load range. (ii) During the operation, balanced excitation is essential to guarantee that the out-of-phase mode remain significantly stronger than the in-phase mode, thus allowing sharp phase locked loop locking and hence robust performance. The proposed model can be used to assess the magnitude of asymmetries introduced by a given manufacturing process and accurately predict the performance of DETF force sensors. For the specific sensor characterized in this study, the proposed model can capture the full dynamic response of the DETF and accurately predict its maximum axial compressive load; by contrast, the conventional single-DOF model does not capture peak splitting and overpredicts the maximum load by ~18%. The proposed model fits the measured frequency response of the electromechanical system and its load-frequency data with coefficient of determination (R2) of 95.4% (0.954) and 99.2% (0.992), respectively.
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Microlattices as Architected Thin Films: Analysis of Mechanical Properties and High Strain Elastic Recovery
K. J. Maloney, C. S. Roper, A. J. Jacobsen, L. Valdevit, W. B. Carter, T. A. Schaedler
APL Materials, 1 (2013) 022106
Abstract
Ordered periodic microlattices with densities from 0.5 mg/cm3 to 500 mg/cm3 are fabricated by depositing various thin film materials (Au, Cu, Ni, SiO2, poly(C8H4F4)) onto sacrificial polymer lattice templates. Young’s modulus and strength are measured in compression and the density scaling is determined. At low relative densities, recov- ery from compressive strains of 50% and higher is observed, independent of lattice material. An analytical model is shown to accurately predict the transition between recoverable “pseudo-superelastic” and irrecoverable plastic deformation for all con- stituent materials. These materials are of interest for energy storage applications, de- ployable structures, and for acoustic, shock, and vibration damping.
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Emergence of film thickness and grain size dependent elastic properties in nanocrystalline thin films
J. Lian, S-W. Lee, L. Valdevit, M. I. Baskes, J. R. Greer
Scripta Materialia, 68 (2013) 261–64
Abstract
Molecular dynamics simulations of nanocrystalline Ni revealed that the in-plane Young’s modulus of 2.2 nm grained Ni film with 10 grains across its thickness was only 0.64% smaller than that of bulk, while it dropped to 24.1% below bulk value for ~1 grain across film. This size dependence arises from the increased number of more compliant grains adjacent to the free surface. Simulations of nanocrystalline diamond revealed that the anharmonicity of the potential curve determined the sensitivity of the Young’s modulus to variations in the sample size.
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Compressive Strength of Hollow Microlattices: Experimental Characterization, Modeling and Optimal Design
L. Valdevit, S. W. Godfrey, T. A. Schaedler, A. J. Jacobsen, W. B. Carter
Journal of Materials Research, Special Issue on Porous Metals, 28 (2013) 2461-2473
Abstract
Recent advances in multiscale manufacturing enable fabrication of hollow-truss based lattices with dimensional control spanning seven orders of magnitude in length scale (from ;50 nm to ;10 cm), thus enabling the exploitation of nano-scale strengthening mechanisms in a macroscale cellular material. This article develops mechanical models for the compressive strength of hollow microlattices and validates them with a selection of experimental measurements on nickel microlattices over a wide relative density range (0.01–10%). The limitations of beam-theory-based analytical approaches for ultralight designs are emphasized, and suitable numerical (finite elements) models are presented. Subsequently, a novel computational platform is utilized to efficiently scan the entire design space and produce maps for optimally strong designs. The results indicate that a strong compressive response can be obtained by stubby lattice designs at relatively high densities (~10%) or by selectively thickening the nodes at ultra-low densities.
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2012

Ultra-high dynamic range resonant MEMS load cells for micromechanical test frames
K. Azgin, T. Akin, L. Valdevit
Journal of Microelectromechanical Systems 21 (2012) 1519-1529
Abstract
This paper presents a resonant double-ended tuning fork (DETF) force sensor with an experimentally demonstrated resolution of 7 nN and a compressive load range of 0.08 N, exceeding a dynamic range of 140 dB (100 parts per billion). The resonator has a scale factor of 216 kHz/N, a Q-factor exceeding 60 000 at 3-mtorr ambient pressure, and a zero-load resonant frequency of 47.6 kHz. The resonator is kept at resonance via a phase-locked loop composed of discrete elements. The sensor is implemented with a silicon-on-glass process with a 100-μm-thick 111 silicon structural layer. The sensor and the complete readout circuit are fully embedded in a compact 65 mm × 52 mm printed circuit board (PCB). The outof-plane parasitic modes of the DETF are also investigated with finite-element simulations and laser Doppler vibrometry experiments, and are verified to be outside of the device working range. The PCB is mounted on a microstage and coupled with an off-the-shelf displacement actuator to realize an economical, versatile, and robust micromechanical test frame with unprecedented combination of force and displacement resolution and range.
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Characterization of nickel-based microlattice materials with structural hierarchy from the nanometer to the millimeter scale
A. Torrents, T. A. Schaedler, A. J. Jacobsen, W. B. Carter, L. Valdevit
Acta Materialia, 60 (2012) 3511-3523
Abstract
Novel nickel-based microlattice materials with structural hierarchy spanning three different length scales (nm, μm, mm) are characterized microstructurally and mechanically. These materials are produced by plating a sacrificial template obtained by self-propagating photopolymer waveguide prototyping. Ni–P films with a thickness of 120 nm to 3 μm are deposited by electroless plating, whereas thicker films (5–26 μm) are obtained by subsequent electrodeposition of a pure Ni layer. This results in cellular materials spanning three orders of magnitude in relative density, from 0.01% to 8.5%. The thin electroless Ni–P films have ultra-fine grain size (7 nm) and a yield strength of ∼2.5 GPa, whereas the thicker electrodeposited Ni films exhibit a much broader distribution with average grain size of 116 nm and strong (1 0 0) texture in the plating direction, resulting in a yield strength of ∼1 GPa. Uniaxial compression experiments reveal two distinct mechanical responses. At ultra-low densities (<0.1%), these lattices exhibit nearly full recovery after strains up to more than 50%, and damping coefficients an order of magnitude larger than for conventional Ni foams. At higher densities (0.1–10%), the compression behavior is fully plastic, similar to traditional cellular metals. A simple mechanical analysis reveals that the transition occurs when the thickness-to-diameter ratio of the truss elements is of the order of the yield strain of the material, in agreement with experimental observations. Optical and electron imaging of deformed lattices show that the deformation largely localizes around the nodes. In the ultra-light regime, the microlattice materials are stiffer and stronger than any existing alternative.
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2011

Ultralight Metallic Microlattices
T. A. Schaedler, A. J. Jacobsen, A. Torrents, A. E. Sorensen, J. Lian, J. R. Greer, L. Valdevit, W. B. Carter
Science, 334 (6058) 962-965 (2011)
Abstract
Ultralight (<10 milligrams per cubic centimeter) cellular materials are desirable for thermal insulation; battery electrodes; catalyst supports; and acoustic, vibration, or shock energy damping. We present ultralight materials based on periodic hollow-tube microlattices. These materials are fabricated by starting with a template formed by self-propagating photopolymer waveguide prototyping, coating the template by electroless nickel plating, and subsequently etching away the template. The resulting metallic microlattices exhibit densities ρ ≥ 0.9 milligram per cubic centimeter, complete recovery after compression exceeding 50% strain, and energy absorption similar to elastomers. Young’s modulus E scales with density as E ~ ρ2, in contrast to the E ~ ρ3 scaling observed for ultralight aerogels and carbon nanotube foams with stochastic architecture. We attribute these properties to structural hierarchy at the nanometer, micrometer, and millimeter scales.
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Protocol for the Optimal Design of Multifunctional Structures: From Hypersonics to Micro-Architected Materials
L. Valdevit, A. J. Jacobsen, J. R. Greer and W. B. Carter
Journal of the American Ceramic Society, Special Issue in Honor of Anthony G. Evans, 94 [S1] (2011), S15-S34
Abstract
Cellular materials with periodic architectures have been extensively investigated over the past decade for their potential to provide multifunctional solutions for a variety of applications, including lightweight thermo-structural panels, blast resistant structures, and high-authority morphing components. Stiffer and stronger than stochastic foams, periodic cellular materials lend themselves well to geometry optimization, enabling a high degree of tailorability and superior performance benefits. This article reviews a commonly established optimal design protocol, extensively adopted at the macro-scale for both single and multifunctional structures. Two prototypical examples are discussed: the design of strong and lightweight sandwich beams subject to mechanical loads and the combined material/ geometry optimization of actively cooled combustors for hypersonic vehicles. With this body of literature in mind, we present a motivation for the development of micro-architected materials, namely periodic multiscale cellular materials with overall macroscopic dimensions yet with features (such as the unit cell or subunit cell constituents) at the micro- or nano-scale. We review a suite of viable manufacturing approaches and discuss the need for advanced experimental tools, numerical models, and optimization strategies. In analyzing challenges and opportunities, we conclude that the technology is approaching maturity for the development of micro-architected materials with unprecedented combinations of properties (e.g., specific stiffness and strength), with tremendous potential impact on a number of fields.
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Mechanical Characterizations of Cast Poly(3,4-ethylenedioxythiophene):Poly(styrenesulfonate)/Polyvinyl Alcohol thin films
C-H. Chen, A. Torrents, L. Kulinsky, R. D. Nelson, M. Madou, L. Valdevit, J.C. LaRue
Synthetic Metals, 161 (2011) 2259-2267
Abstract

The polymer Poly(3,4-ethylenedioxythiophene):Poly(styrenesulfonate), hereafter referred to as PEDOT:PSS, has electrical properties superior to those of most conducting polymers, but it is too brittle to be employed in many applications. Blending PEDOT:PSS with other polymers is a promising route to reach a good trade-off between electrical and mechanical properties. This paper describes the mechanical characterization of PEDOT:PSS/PVA (Polyvinyl Alcohol) blends. The PEDOT:PSS/PVA films used in this study are produced by casting, and uniaxial tensile tests are performed to characterize the Young’s modulus, fracture strain, tensile strength, and plastic deformation behavior of the blends as a function of the weight fraction of the components. For pure PVA, the Young’s modulus, fracture strain and tensile strength are found to be, respectively, 41.3 MPa, 111% and 41.3 MPa. The strength exhibits a nearly perfect bimodal behavior, suddenly increasing by a factor 2 at a PEDOT:PSS content of 30%. Importantly, the ductility remains extremely high (∼94%, only 20% lower than pure PVA) up to PEDOT:PSS fractions of ∼50%. The Young’s modulus monotonically increases with PEDOT:PSS content, reaching 1.63 GPa at 50%. SEM imaging and XRD analysis allows correlation of these evolutions to substantial morphological changes in the PEDOT:PSS/PVA microstructure. When combined with a previously published electrical characterization study, the current work suggests that a PEDOT:PSS/PVA polymer blend with 30–40 wt% of PEDOT:PSS provides the best trade-off of conductivity and ductility. For non free-standing films, higher PEDOT:PSS fractions (70%) might be preferable.

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Implications of Shakedown for Design of Actively-Cooled Thermostructural Panels
N. Vermaak, L. Valdevit, A. G. Evans, F. W. Zok and R. M. McMeeking
Journal of the Mechanics of Materials and Structures 6 (2011) 1313-1327
Abstract
Propulsion systems in future hypersonic vehicles will require use of actively cooled structures that can withstand extreme thermomechanical loads. Candidate designs and materials for such structures have previously been identified through conventional yield-based design principles. The present article out- lines an approach that utilizes concepts of localized plasticity and shakedown under cyclic loading in the design process. For this purpose, an established computational technique is used to determine shakedown limits for prototypical cooled structures. The results are employed in a design sensitivity study. The study demonstrates that, by allowing for shakedown, structures with areal densities significantly lower than those obtained from yield-limited design can be obtained. The magnitude of the benefits depends on the specific geometry of interest, the thermomechanical boundary conditions and the constraints placed on the design.
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Concentration independent modulation of local micromechanics in a fibrin clot
M. A. Kotlarchyk, S. G. Shreim, M. B. Alvarez-Elizondo, L. C. Estrada, R. Singh, L. Valdevit, E. Kniazeva, E. Gratton, A. J. Putnam and E. L. Botvinick
PLoS ONE, 6 (2011) e20201
Abstract
Methods for tuning extracellular matrix (ECM) mechanics in 3D cell culture that rely on increasing the concentration of either protein or cross-linking molecules fail to control important parameters such as pore size, ligand density, and molecular diffusivity. Alternatively, ECM stiffness can be modulated independently from protein concentration by mechanically loading the ECM. We have developed a novel device for generating stiffness gradients in naturally derived ECMs, where stiffness is tuned by inducing strain, while local mechanical properties are directly determined by laser tweezers based active microrheology (AMR). Hydrogel substrates polymerized within 35 mm diameter Petri dishes are strained non-uniformly by the precise rotation of an embedded cylindrical post, and exhibit a position-dependent stiffness with little to no modulation of local mesh geometry. Here we present the device in the context of fibrin hydrogels. First AMR is used to directly measure local micromechanics in unstrained hydrogels of increasing fibrin concentration. Changes in stiffness are then mapped within our device, where fibrin concentration is held constant. Fluorescence confocal imaging and orbital particle tracking are used to quantify structural changes in fibrin on the micro and nano levels respectively. The micromechanical strain stiffening measured by microrheology is not accompanied by ECM microstructural changes under our applied loads, as measured by confocal microscopy. However, super-resolution orbital tracking reveals nanostructural straightening, lengthening, and reduced movement of fibrin fibers. Furthermore, we show that aortic smooth muscle cells cultured within our device are morphologically sensitive to the induced mechanical gradient. Our results demonstrate a powerful cell culture tool that can be used in the study of mechanical effects on cellular physiology in naturally derived 3D ECM tissues.
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Catastrophic vs. gradual collapse of thin-walled nanocrystalline Ni cylinders as building blocks of micro-lattice structures
J. Lian, L. Valdevit, T. A. Schaedler, A. J. Jacobsen, W. B. Carter and J. R. Greer
Nano Letters, 11 (2011) 4118-4125
Abstract
Lightweight yet stiff and strong lattice structures are attractive for various engineering applications, such as cores of sandwich shells and components designed for impact mitigation.
Recent breakthroughs in manufacturing enable efficient fabrication of hierarchically architected microlattices, with dimensional control spanning seven orders of magnitude in length scale. These materials have the potential to exploit desirable nanoscale-size effects in a macroscopic structure, as long as their mechanical behavior at each appropriate scale nano, micro, and macro levels is properly understood. In this letter, we report the nanomechanical response of individual microlattice members. We show that hollow nanocrystalline Ni cylinders differing only in wall thicknesses, 500 and 150 nm, exhibit strikingly different collapse modes: the 500 nm sample collapses in a brittle manner, via a single strain burst, while the 150 nm sample shows a gradual collapse, via a series of small and discrete strain bursts. Further, compressive strength in 150 nm sample is 99.2% lower than predicted by shell buckling theory, likely due to localized buckling and fracture events observed during in situ compression experiments. We attribute this difference to the size-induced transition in deformation behavior, unique to nanoscale, and discuss it in the framework of “size effects” in crystalline strength.
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2010

Pressure Induced Amorphization in Silicon Caused by the Impact of Electrosprayed Nanodroplets
M. Gamero-Castano, A. Torrents, L. Valdevit, J-G. Zheng
Physical Review Letters 105 (2010) 145701
Abstract
This Letter describes the shock-induced amorphization of single-crystal Si bombarded by nanodroplets. At impact velocities of several kilometers per second, the projectiles trigger strong compression pulses lasting tens of picoseconds. The phase transition, confirmed via transmission electron microscopy and electron backscatter diffraction, takes place when the projectile’s stagnation pressure is approximately 15 GPa. We speculate that the amorphization results either from the decompression of the beta-Sn phase or during the compression of the diamond phase.
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MEMS resonant load cells for micro-mechanical test frames: Feasibility study and optimal design
A. Torrents, K. Azgin, S. W. Godfrey, E. S. Topalli, T. Akin, L. Valdevit
Journal of Micromechanics and Microengineering, 20 (2010) 125004 (17pp)
Abstract
This paper presents the design, optimization and manufacturing of a novel micro-fabricated load cell based on a double-ended tuning fork. The device geometry and operating voltages are optimized for maximum force resolution and range, subject to a number of manufacturing and electromechanical constraints. All optimizations are enabled by analytical modeling (verified by selected finite elements analyses) coupled with an efficient C++ code based on the particle swarm optimization algorithm. This assessment indicates that force resolutions of ∼0.5–10 nN are feasible in vacuum (∼1–50 mTorr), with force ranges as large as 1 N. Importantly, the optimal design for vacuum operation is independent of the desired range, ensuring versatility. Experimental verifications on a sub-optimal device fabricated using silicon-on-glass technology demonstrate a resolution of ∼23 nN at a vacuum level of ∼50 mTorr. The device demonstrated in this article will be integrated in a hybrid micro-mechanical test frame for unprecedented combinations of force resolution and range, displacement resolution and range, optical (or SEM) access to the sample, versatility and cost.
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Influence of Configuration on Materials Selection for Actively-Cooled Combustors
N. Vermaak, L. Valdevit, A. G. Evans, F. W. Zok and R. M. McMeeking
AIAA Journal of Propulsion and Power 26 (2010) 295-302
Abstract
The influence of combustor size and shape on material feasibility is explored using (structural and fuel) weight, as well as fuel economy as metrics. A materials selection methodology developed for actively cooled rectangular panels has been embellished to include cylindrical/annular configurations. The procedure incorporates an analytical model for temperature and stress distributions subject to thermomechanical loads representative of hypersonic flight conditions. The model has been numerically verified using finite element simulations. By combining the model with optimization routines, materials robustness maps have been produced, depicting the range of thermal loads and fuel flow rates that satisfy all design constraints. A wide selection of high-temperature materials has been investigated. Comparisons of cylindrical and rectangular combustors are made for the leading candidates. It is established that the cylindrical designs allow both lighter optimal structures as well as greater robustness and fuel economy.
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2009

Materials Property Profiles for Actively Cooled Panels: An Illustration for Scramjet Applications
N. Vermaak, L. Valdevit, A.G. Evans
Metallurgical and Materials Transactions A 40A (2009) 877-890
Abstract
A scheme for identifying and visualizing the material properties that limit the performance of candidate materials for actively cooled aerospace propulsion components is presented and illustrated for combustor panels for Mach 7 hypersonic vehicles. The method provides a framework for exploring the nonlinear interactions between design and materials optimization. By probing the active constraints along the border of feasible design space, the limiting properties have been elucidated for a representative group of candidate materials. Property vectors that enhance design options have also been determined. For one of the promising candidate alloys (the Ni-based superalloy, INCONEL X-750), the possibilities of reclaiming design space and lowering optimal combustor panel weight by tailoring its strength properties are assessed.
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Feasibility of metallic structural heat pipes as sharp leading edges for hypersonic vehicles
C. Steeves, M.Y. He, S.D. Kasen, L. Valdevit, H.N.G. Wadley and A.G. Evans
Journal of Applied Mechanics 76 (2009) 031014 (9p)
Abstract
The influence of combustor size and shape on material feasibility is explored using (structural and fuel) weight, as well as fuel economy as metrics. A materials selection methodology developed for actively cooled rectangular panels has been embellished to include cylindrical/annular configurations. The procedure incorporates an analytical model for temperature and stress distributions subject to thermomechanical loads representative of hypersonic flight conditions. The model has been numerically verified using finite element simulations. By combining the model with optimization routines, materials robustness maps have been produced, depicting the range of thermal loads and fuel flow rates that satisfy all design constraints. A wide selection of high-temperature materials has been investigated. Comparisons of cylindrical and rectangular combustors are made for the leading candidates. It is established that the cylindrical designs allow both lighter optimal structures as well as greater robustness and fuel economy.
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2008

Organic substrates for flip chip design: a thermo-mechanical model that accounts for heterogeneity and anisotropy
L. Valdevit, V. Khanna, A. Sharma, S. Sri-Jayantha, D. Questad, K. Sikka
Microelectronics Reliability, 48 (2008), 245-260
Abstract
We present a thermo-mechanical characterization of organic substrates that accounts for heterogeneity both in the in-plane and out-of-plane directions. Systematic observation of the board files of a number of substrates of commercial interest reveals primarily three recurrent topological arrangements of copper and polymer; for each arrangement, the in-plane effective thermo-elastic properties are calculated via appropriate composite materials models. The averaging process in the out-of-plane direction (i.e. the stacking effect) is performed using standard laminated plate theory. The model is successfully applied to various regions of three organic substrates of interest (mainly differing in core thickness): the analytically calculated effective Young’s moduli (E) and coefficients of thermal expansion (CTE) are shown to be typically within 10% of the experimental measurements. An important attribute of this model is its ability to provide substrate description at various levels of complexity: a few effective properties are outputted that can be useful for further purely analytical investigations; at the same time, the model provides the full stiffness matrix for each region of the substrate, to be used for more detailed finite elements simulations of higher-level structures (e.g. silicon die/underfill/substrate/cooling solution assemblies). Preliminary application of this model to the warp analysis of a flip-chip is presented in the end.
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A materials selection protocol for lightweight actively cooled panels
L. Valdevit, N. Vermaak, F. W. Zok, A. G. Evans
Journal of Applied Mechanics 75 (2008) 061022 (15p)
Abstract
This article provides a materials selection methodology applicable to lightweight actively cooled panels, particularly suitable for the most demanding aerospace applications. The key ingredient is the development of a code that can be used to establish the capabilities and deficiencies of existing panel designs and direct the development of advanced materials. The code is illustrated for a fuel-cooled combustor liner of a hypersonic vehicle, optimized for minimum weight subject to four primary design constraints (on stress, temperatures, and pressure drop). Failure maps are presented for a number of candidate high-temperature metallic alloys and ceramic composites, allowing direct comparison of their thermostructural performance. Results for a Mach 7 vehicle under steady-state flight conditions and stoichiometric fuel combustion reveal that, while C–SiC satisfies the design requirements at minimum weight, the Nb alloy Cb752 and the Ni alloy Inconel X-750 are also viable candidates, albeit at about twice the weight. Under the most severe heat loads (arising from heat spikes in the combustor), only Cb752 remains viable. This result, combined with robustness benefits and fabrication facility, emphasizes the potential of this alloy for scramjets. 
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2007

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2006

Structural performance of near-optimal sandwich panels with corrugated cores
L. Valdevit, Z. Wei, C. Mercer, F. W. Zok, A. G. Evans
International Journal of Solids and Structures, 43 (2006), 4888-4905
Abstract
An experimental and computational study of the bending response of steel sandwich panels with corrugated cores in both transverse and longitudinal loading orientations has been performed. Panel designs were chosen on the basis of failure mechanism maps, constructed using analytic models for failure initiation. The assessment affirms that the analytic models provide accurate predictions when failure initiation is controlled by yielding. However, discrepancies arise when failure initiation is governed by other mechanisms. One difficulty is related to the sensitivity of the buckling loads to the rotational constraints of the nodes, as well as to fabrication imperfections. The second relates to the compressive stresses beneath the loading platen. To address these deficiencies, existing models for core failure have been expanded. The new results have been validated by experimental measurements and finite element simulations. Limit loads have also been examined and found to be sensitive to the failure mechanism. When face yielding predominates, appreciable hardening follows the initial non-linearity, rendering robustness. Conversely, for designs controlled by buckling (either elastic or plastic) failure initiation is immediately followed by softening. The implication is that, when robustness is a key requirement, designs within the face failure domain are preferred.
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Optimal active cooling performance of metallic sandwich panels with prismatic cores
L. Valdevit, A. Pantano, H. A. Stone, A. G. Evans
Int. Journal of Heat and Mass Transfer, 49 (2006), 3819-3830
Abstract
All-metallic sandwich panels with prismatic cores are being currently investigated for combined structural and active cooling performance. We present a new approach to active cooling performance, and use it to optimize the panel geometry for four different systems: aluminum-air, aluminum-water, aluminum-gasoline and titanium-gasoline. The results show that some geometric parameters can be fixed without much detriment in thermal performance. Moreover, while optimal core densities are typically 25–50%, near-optimal results can be obtained with densities as low as 10%. These findings provide considerable geometric flexibility when attempting combined thermal and structural optimization.
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2005

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2004

Structurally optimized sandwich panels with prismatic cores
L. Valdevit, J. W. Hutchinson, A. G. Evans
International Journal of Solids and Structures, 41 (2004), 5105-5124
Abstract
Multifunctional sandwich panels with corrugated and prismatic diamond cores have been analyzed and their behavior compared with panels designed using truss and honeycomb cores. Failure mechanism maps have been devised that account for interactions between core and face members during buckling. The optimal dimensions and the minimum weight have been evaluated. The load capacities predicted for near-optimal designs have been validated by conducting selected finite element calculations. Designs that use diamond prismatic cores (with corrugation order 4) are slightly more weight efficient than trusses, when optimized for a specific loading direction. Honeycomb cores, while somewhat more weight efficient, especially at lower load capacities, are not amenable to the fluid flows needed for cooling. We conclude that the diamond prismatic topology is the most weight efficient among designs amenable to simultaneous load bearing and active cooling.
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Active cooling by metallic sandwich structures with periodic cores
T. J. Lu, L. Valdevit, A. G. Evans
Progress in Materials Science, 50 (2004), 789-815
Abstract
We review the thermal characteristics of all-metallic sandwich structures with two dimensional prismatic and truss cores. Results are presented based on measurements in conjunction with analytical modeling and numerical simulation. The periodic nature of these core structures allows derivation of the macroscopic quantities of interest—namely, the overall Nusselt number and friction factor—by means of correlations derived at the unit cell level. A fin analogy model is used to bridge length scales. Various measurements and simulations are used to examine the robustness of this approach and the limitations discussed. Topological preferences are addressed in terms scaling relations obtained with three dimensionless parameters—friction factor, Nusselt number and Reynolds number—expressed both at the panel and the cell levels. Countervailing influences of topology on the Nusselt number and friction factor are found. Case studies are presented to illustrate that the topology preference is highly application dependent.
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