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A 3D-Printed Molecular Ferroelectric Metamaterial A 3D-printed molecular ferroelectric metamaterial Yong Hua,1, Zipeng Guob,1, Andrew Ragonesea,1, Taishan Zhuc, Saurabh Khujea, Changning Lia, Jeffrey C. Grossmanc, Chi Zhoub,2, Mostafa Nouha,2, and Shenqiang Rena,d,e,2 aDepartment of Mechanical and Aerospace Engineering, The State University of New York at Buffalo, Buffalo, NY 14260; bDepartment of Industrial and Systems Engineering, The State University of New York at Buffalo, Buffalo, NY 14260; cDepartment of Materials Science and Engineering, Massachusetts Institute of Technology, Cambridge, MA 02139; dDepartment of Chemistry, The State University of New York at Buffalo, Buffalo, NY 14260; and eResearch and Education in Energy Environment & Water Institute, The State University of New York at Buffalo, Buffalo, NY 14260 Edited by Thomas E. Mallouk, University of Pennsylvania, University Park, PA, and approved September 21, 2020 (received for review July 2, 2020) Molecular ferroelectrics combine electromechanical coupling and high loading of solid functional component is required to afford electric polarizabilities, offering immense promise in stimuli- functionalities in printed structures (19), while this challenges the dependent metamaterials. Despite such promise, current physical homogeneity and viscosity stability for ultimate printability of the realizations of mechanical metamaterials remain hindered by the feedstock. Additive manufacturing and its design space in func- lack of rapid-prototyping ferroelectric metamaterial structures. tional ferroelectric materials are particularly limited due to the Here, we present a continuous rapid printing strategy for the vol- limitation of ferroelectric solid component loading. In addition, the umetric deposition of water-soluble molecular ferroelectric meta- mechanical flexibility and ferroelectricity of printed materials are materials with precise spatial control in virtually any three- diminished as a result of randomly organized components (20, 21). dimensional (3D) geometry by means of an electric-field–assisted Therefore, a seamless integration of additive manufacturing, mo- additive manufacturing. We demonstrate a scaffold-supported lecular ferroelectric materials, and metamaterial design would ferroelectric crystalline lattice that enables self-healing and a provide the ultimate solution to unlock the functional material and reprogrammable stiffness for dynamic tuning of mechanical exotic structural properties of molecular ferroelectric metamaterials metamaterials with a long lifetime and sustainability. A molecu- for unprecedented emerging applications. lar ferroelectric architecture with resonant inclusions then ex- Here, we unravel a printable mechanical metamaterial of imi- hibits adaptive mitigation of incident vibroacoustic dynamic dazolium perchlorate (ImClO4) (2, 22, 23), a transparent molec- loads via an electrically tunable subwavelength-frequency band ular ferroelectric with superior electromechanical coupling and gap. The findings shown here pave the way for the versatile ad- reprogrammable stiffness. We propose a continuous rapid 3D ENGINEERING ditive manufacturing of molecular ferroelectric metamaterials. printing technique which can reduce the manufacturing time of ferroelectrics from hours down to minutes. Different from con- molecular ferroelectrics | mechanical metamaterials | hydrogel | additive ventional inorganic or organic–inorganic ferroelectrics (24, 25), manufacturing | three-dimensional printing the ionic nature of molecular ferroelectrics enables high solu- bility in water, ensuring a highly dense and transparent precur- olution-processable molecular ferroelectrics, which show sor. We optically pattern the 3D architecture scaffolds through Sferroelectric properties approaching inorganic perovskites, have amassed much recent attention due to their lightweight, Significance tunable electrooptic and electromechanical coupling effects (1–5). Spontaneous polarization and the ability to switch the electromechanical activity by an external electric or mechanical Molecular ferroelectrics, which show the ability to switch the stimulus is of prime importance, establishing the basis for many electromechanical activity by an external electric field, estab- metamaterial technologies (6–8). Over the past decade, elastic lish the basis for mechanical metamaterial technologies. De- metamaterials with resonant inclusions have gained significant spite their theoretical promise, such mechanical metamaterials remain hindered by the lack of adaptive stimuli-responsive traction owing to their unique response to incident dynamic “ ” loads, ranging from subwavelength band gaps (9–11), back- materials which can be effectively tuned on demand across scattering immune wave guides (12, 13), and topological time and length scales. Here, we unravel a printable mechani- pumps (14–16), to the design of logic gates, nonreciprocity, and cal metamaterial of imidazolium perchlorate with superior diodelike formations (17, 18). Despite their theoretical promise, electromechanical coupling and reprogrammable stiffness. We such mechanical metamaterials remain hindered by the lack of propose a continuous rapid three-dimensional (3D) printing technique which can reduce the manufacturing time of ferro- adaptive stimuli-responsive materials which can be effectively electrics from hours down to minutes. The printed molecular tuned “on demand” across the time and length scales dictated by ferroelectric metamaterial structure is then shown to enable a such metamaterials. On the other hand, heterogeneous meta- tunable-frequency vibration-isolating architecture. This study material structures and systems have been shown to produce paves the way for rationally designed 3D-printable molecular tailorable properties beyond those of the constitutive materials ferroelectric metamaterials. (ferroelectrics) owing to the unique geometrical and topological material reorganization. However, the hallmark feature of such Author contributions: Y.H., Z.G., A.R., C.Z., M.N., and S.R. designed research; Y.H., Z.G., metamaterials is a hierarchical architecture which often exhibits A.R., and T.Z. performed research; Y.H., Z.G., A.R., C.L., T.Z., and J.C.G. contributed new highly complicated internal features, rendering these exotic reagents/analytic tools; Y.H., Z.G., A.R., T.Z., C.Z., and M.N. analyzed data; and Y.H., Z.G., structures extremely challenging, if not impossible, to achieve A.R., T.Z., S.K., J.C.G., C.Z., M.N., and S.R. wrote the paper. with traditional manufacturing processes. The authors declare no competing interest. Three-dimensional (3D) printing has been hailed as an emerging This article is a PNAS Direct Submission. advanced manufacturing paradigm, providing a large potential to Published under the PNAS license. rapidly fabricate highly complicated metamaterial structures with a 1Y.H., Z.G., and A.R. contributed equally to this work. wide variety of materials owing to its elegant concept of layer by 2To whom correspondence may be addressed. Email: [email protected], mnouh@ layer deposition. However, 3D printing is mainly limited to creating buffalo.edu, or [email protected]. complex geometries of nonfunctional structures. The competition This article contains supporting information online at https://www.pnas.org/lookup/suppl/ between printability and functionality has been identified as the doi:10.1073/pnas.2013934117/-/DCSupplemental. main limitation of 3D printing in functional materials. Generally, a www.pnas.org/cgi/doi/10.1073/pnas.2013934117 PNAS Latest Articles | 1of7 Downloaded by guest on September 29, 2021 stereolithography (SLA) 3D printing for selective volumetric desired ferroelectric performance by changing the concentration crystallization of ionic ImClO4 precursor. The SLA-printed water- of ImClO4 or the ratio of PEGDA. Thus, we prepare the pre- soluble ferroelectric precursor and photopolymerizable material cursor with saturated ImClO4 solution and low volume ratio of with a highly porous yet tough polymer network serve as an ex- PEGDA (5 vol %). Finally, dried printed samples with around cellent carrier to in situ crystalize and organize molecular ferro- 50 vol% ratio of ImClO4 are obtained. electric crystals. The patterned scaffold is then dehydrated under a In general, the crystal growth in a liquid environment is con- biased electric field to crystallize ImClO4 with the desired polar- trolled by two processes: the diffusion of ions through the liquid ization orientation. The printed molecular ferroelectrics also ex- phase to the growth front and the reorganization of crystal grains hibit a self-healing ability from the overloaded mechanical and into the polycrystal. In our experiments, the diffusion of ions electric field (26, 27). The printed molecular ferroelectric meta- should not be the limiting factor because of the highly concen- material structure is then shown to enable a tunable-frequency trated ImClO4 precursor solution and large pore size of the vibration-isolating architecture. This study paves the way for ra- hydrogel scaffold. Thus, the crystal grain reorganization is the tionally designed 3D-printable molecular ferroelectric materials limiting step during the growth. By applying a biased electric for mechanical metamaterials. field, we can organize the orientation of small grains formed C Results right after the nucleation. As shown in Fig. 1 , the dehydration process was conducted under an electric field, which was applied 3D Fabrication Process. Three-dimensional SLA printing enables to obtain
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