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In-Situ Mechanics of 3D Graphene Foam Based Ultra-Stiff and Flexible

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In-Situ Mechanics of 3D Graphene Foam Based Ultra-Stiff and Flexible Carbon 137 (2018) 502e510 Contents lists available at ScienceDirect Carbon journal homepage: www.elsevier.com/locate/carbon In-situ mechanics of 3D graphene foam based ultra-stiff and flexible metallic metamaterial * Pranjal Nautiyal a, Mubarak Mujawar b, Benjamin Boesl a, Arvind Agarwal a, a Nanomechanics and Nanotribology Laboratory, Department of Mechanical and Materials Engineering, Florida International University, 10555 West Flagler Street, Miami, FL 33174, USA b Advanced Materials Engineering Research Institute, Florida International University, 10555 West Flagler Street, Miami, FL 33174, USA article info abstract Article history: A 3D macroporous graphene foam based ultra-lightweight, stiff and fatigue-resistant mechanical met- Received 7 April 2018 amaterial is developed in this study. In-situ indentation of the 3D graphene framework reveals an Received in revised form extraordinary spring constant of ~15 N/m and an upward of 70% recoverable deformation. The brilliant 19 May 2018 stiffness and superelasticity of graphene foam is exploited to fabricate Aluminum-based Graphene/Metal Accepted 28 May 2018 Metamaterial by electron beam evaporation. In-situ cyclic indentation inside SEM up to 50 cycles Available online 29 May 2018 revealed long-distance stress-transfer due to the interconnected network of branches, having spring-like mechanical energy storage ability. The structure is highly fatigue-resistant, with more than 98% of displacement recovery at the end of each loading/unloading cycle. In-situ tensile investigation reveals shearing-type failure with dual-strengthening mechanisms, where stress transfer from Aluminum layer to graphene scaffold enhances the overall load bearing ability and the Aluminum deposit on graphene foam provides a structural backbone that restricts brittle failure. A modified scaling law is proposed for modeling the mechanical strength of cellular metamaterials that takes into consideration the hollow anatomy of graphene frameworks, thereby bridging the current gap in theoretical and experimental foam mechanics. The 3D metamaterial developed in this study can be a game-changing candidate for developing flyweight metallic structures with unprecedented elasticity, stiffness and fatigue-resistance. © 2018 Elsevier Ltd. All rights reserved. 1. Introduction engineering structural materials with brilliant mechanical proper- ties. Nano-structured materials, such as nanocrystals, nanofibers, In recent years, controlled and rational design of material ar- nanoparticles, nanotubes and nanosheets display remarkable me- chitectures has taken a center stage in materials science as a chanical stiffness and strength and hence, have attracted attention strategy to achieve desired functionalities in metamaterials [1e5]. as filler materials for lightweight structural metals to augment their These metamaterials comprise of repeating unit cells and their mechanical properties [10e12]. However, this approach does not properties are strongly correlated to their structure rather than the provide desired microstructure control and introduces structural composition. Mechanical metamaterials have gained traction for defects, resulting in unwarranted variability in properties and developing lightweight, stable and strong structures by carefully performance. To overcome this challenge, carefully designed met- controlling the architecture [6,7]. From structural application amaterials made from the desired nano-structured materials can be standpoint, low density cellular or porous architectures are highly employed as fillers for obtaining homogeneous material micro- preferable. ‘Free-standing’ mechanical metamaterials are able to structures. Graphene is a well-known two-dimensional nano- effectively translate excellent material properties at nanoscale to material, with an excellent in-plane elastic modulus as high as achieve desirable mechanical attributes at macroscale [8,9]. 1 TPa and a tensile strength of 130 GPa [13]. These mechanical Combining the metamaterial design approach with excellent properties of graphene make it a promising material candidate for ‘intrinsic’ material properties can be a highly effective strategy for developing cellular mechanical metamaterials [14]. There has been tremendous interest in 3D frameworks of gra- phene in recent years. Some of the examples of popular graphene * Corresponding author. architectures from application standpoint are hydrogel, aerogel, E-mail address: agarwala@fiu.edu (A. Agarwal). cork, macroporous foam, and nanoporous sponge [15]. These https://doi.org/10.1016/j.carbon.2018.05.063 0008-6223/© 2018 Elsevier Ltd. All rights reserved. P. Nautiyal et al. / Carbon 137 (2018) 502e510 503 graphene assemblies are capable of withstanding > 50,000 times lightweight graphene/metal metamaterial (GMM) based on mac- their weight and are characterized by an outstanding recovery from roporous 3D graphene foam and Aluminum in this study. 80% compressed state [16]. Due to their superior specific tensile strength and Young's modulus, 3D graphene monoliths are capable 2. Experimental of energy dissipation with reported energy loss coefficients as high as 87%. Freestanding 3D graphene foam with macroporous archi- 2.1. Fabrication of 3D metamaterial tecture has been demonstrated to be an excellent candidate for applications in structural materials [17], supercapacitors [18], strain The free-standing macroporous 3D graphene foam used in this sensors [19], electromagnetic interference shielding [20], tissue study was obtained from Graphene Supermarket (Calverton, NY, engineering [21], damping [22], de-icing [23] and thermal interface USA). 1 mm thick layer of Al was deposited on graphene foam using material [24]. The interconnected network of hollow branches CHA SAP 600 e-Beam Evaporation system (California, USA). The makes the mechanics of graphene foam unique. During compres- graphene foam was mounted on a quartz substrate and placed in sive loading, the graphene foam undergoes a three-stage defor- the evaporator. Prior to deposition, the system was evacuated to a À mation [25]. At very low strains (ε < 0.1), elastic bending of base pressure of 5 Â 10 7 Torr. 99.99% pure Al target was bom- graphitic ligaments takes place resulting in a linear stress-strain barded with an electron beam (10 kV, 330 mA) to achieve a depo- À regime. At intermediate strains, the plastic collapse of these liga- sition rate of 1 nm/s at an operating pressure of 1 Â 10 6 Torr. The ments results in a plateau in the stress-strain behavior, followed by thickness of the Al deposition was monitored using a quartz crystal a steep rise in stress as a result of compaction of the fragmented monitor. ligaments. Bending, self-folding, and rotation of graphene flakes are proposed as the micromechanisms during plastic deformation [26]. 2.2. In-situ mechanical investigations These micromechanisms can be altered by controlling the stiffness of foam branches, suggesting a tunable Poisson's ratio of 3D gra- For nanoindentation characterizations, the free-standing 3D phene foam. Localized indentation loading of the foam causes the graphene foam (GrF) and Al/GrF metamaterial were mounted on bending of branches, followed by depression of the foam wall at the stage of SEM Picoindenter (Hysitron PI 87, Minnesota, USA). The higher loads [27]. During indentation, the area of interaction be- stage was installed inside a dual beam JEOL JIB-4500 focused ion tween the indenter tip and the foam wall determines the nature of beam/SEM system. A diamond Berkovich tip of 100 nm diameter deformation. Nieto and co-workers reported depression of foam was used to apply localized loads and real-time deformation videos wall upon indentation by conospherical probe, which manifests as were captured by the SEM. Quasi-static nanoindentation tests were an increase in slope of the load-displacement curve [27]. This performed by programming the peak load of 2000 mN and the regime was absent when a flat punch was used to apply the loads loading/unloading rate of 25 mN/s. For fatigue tests, a total of 50 due to greater area and lower stress. Tensile deformation of gra- cycles were performed and the corresponding load-displacement- phene foam causes the branches to align along the loading direc- time profiles were captured. In order to visualize the deformation tion. Due to this alignment, the superior in-plane stiffness and in the materials, microstructural strain analysis of the real-time strength of graphene is utilized to provide enhanced load bearing SEM videos was performed using VIC-2D digital image correlation ability [27]. Due to its hierarchical structure, graphene foam ex- (DIC) software (Correlated Solutions, Irmo, USA). The resultant DIC hibits multi-scale energy dissipation/dispersion mechanisms, such strain maps provide information about the dispersion/transfer of as formation of dynamic ripples, interlayer spring-like van der deformation in the 3D architecture. Waals interactions, kink band formation and hollow wall vibration effect [28]. 3. Results and discussion These observations suggest that graphene foam architecture is structurally robust and highly flexible. We envisage the application 3.1. In-situ mechanics of 3D graphene framework of this unique 3D scaffold for engineering flexible graphene-metal heterostructures. Lightweight metallic microlattices (with achiev- The 3D graphene foam used in this study was obtained by able densities less than 10 mg/cm3) are characterized by efficient chemical vapor deposition of graphene on a Nickel foam. This
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