Microporous and Flexible Framework Acoustic Metamaterials for

Subscriber access provided by AUSTRALIAN NATIONAL UNIV

Letter

Microporous and Flexible Framework Acoustic Metamaterials for Sound Attenuation and Contrast Agent Applications Quin R.S. Miller, Satish K Nune, Herbert Todd Schaef, Ki Won Jung, Kayte M Denslow, Matthew S Prowant, Paul F Martin, and B. Peter McGrail ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.8b19249 • Publication Date (Web): 13 Dec 2018 Downloaded from http://pubs.acs.org on December 15, 2018

Just Accepted “Just Accepted” manuscripts have been peer-reviewed and accepted for publication. They are posted online prior to technical editing, formatting for publication and author proofing. The American Chemical Society provides “Just Accepted” as a service to the research community to expedite the dissemination of scientific material as soon as possible after acceptance. “Just Accepted” manuscripts appear in full in PDF format accompanied by an HTML abstract. “Just Accepted” manuscripts have been fully peer reviewed, but should not be considered the official version of record. They are citable by the Digital Object Identifier (DOI®). “Just Accepted” is an optional service offered to authors. Therefore, the “Just Accepted” Web site may not include all articles that will be published in the journal. After a manuscript is technically edited and formatted, it will be removed from the “Just Accepted” Web site and published as an ASAP article. Note that technical editing may introduce minor changes to the manuscript text and/or graphics which could affect content, and all legal disclaimers and ethical guidelines that apply to the journal pertain. ACS cannot be held responsible for errors or consequences arising from the use of information contained in these “Just Accepted” manuscripts.

is published by the American Chemical Society. 1155 Sixteenth Street N.W., Washington, DC 20036 Published by American Chemical Society. Copyright © American Chemical Society. However, no copyright claim is made to original U.S. Government works, or works produced by employees of any Commonwealth realm Crown government in the course of their duties.

Page 1 of 9 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

ACS Applied Materials & Interfaces

Microporous and Flexible Framework Acoustic Metamaterials for Sound Attenuation and Contrast Agent Applications Quin R.S. Miller 1*, Satish K. Nune 2, H. Todd Schaef 1, Ki Won Jung 2†, Kayte M. Denslow 3, Matthew S. Prowant 3, Paul F. Martin 2, B. Peter McGrail 2 1Physical

and Computational Sciences Directorate, Pacific Northwest National Laboratory, Richland, Washington 99356, United States 2Energy and Environment Directorate, Pacific Northwest National Laboratory, Richland, Washington 99356, United States 3National Security Directorate, Pacific Northwest National Laboratory, Richland, Washington 99356, United States Keywords: low frequency, MOF, metamaterial, acoustic, seismic, contrast agent ABSTRACT: The low-frequency (100-1250 Hz) acoustic properties of metal-organic framework (MOF) materials were examined in impedance tube experiments. The anomalously-high sound transmission loss of HKUST-1, FeBTC, and MIL-53(Al) quantitatively demonstrated that these prototypical MOFs are absorptive acoustic metamaterials. To the best of our knowledge this is the first example of MOFs that have been demonstrated to be acoustic metamaterials. The low-frequency acoustic dampening by subwavelength MOF metamaterials is likely due to sound dissipation and absorption facilitated by multiple internal reflections within the microporous framework structure. Modification of MIL-53(Al) with flexible organic linkers clarified that acoustic signatures of the metal-organic frameworks may be tailored to add or alter certain diagnostic acoustic signatures. These results may be applied to the rational design of lightweight soundinsulating construction materials and acoustic contrast agents for subsurface mapping and monitoring applications at low frequency (100-1250 Hz).

Low-frequency (14 were then hydraulically pressed into 100 mm diameter discs dB and >8 dB underperformance for the basalt and silica samples, (Figure 1) with negligible changes to the MOF crystallites (Figure respectively. The poor experimental TL performance of the rock S1). Acoustic experiments were conducted on the discs using an discs compared to mass law predictions can be fairly typical for impedance tube (Figure 1) with which the normal incidence TL is natural materials, due to the abundance of macroporosity.29 The measured for a sample over a 100-1250 Hz frequency range, MOFs have resonant signatures and anomalous absorbance that according to standardized procedures. 27 The TL is the measure of clearly contrast with representative prototypical geomaterials how much sound energy is attenuated by the sample in terms of the abundant in sedimentary and igneous subsurface environments. redirection of the energy by the material and the absorption of the Enhanced sound adsorption at lower frequencies compared to rock energy within it. samples (i.e. building stone) is also promising for construction material applications. Figure 2a illustrates the normal incidence transmission loss results determined experimentally with the acoustic impedance tube for the four different unmodified MOF samples. The mass law (Equation 1) predictions of TL are also plotted for comparison. Noticeable dips in TL due to the resonances of the MOFs occurred at 160, 225, 200, and 315 Hz for HKUST-1, FeBTC, Ni-MOF-74, and MIL-53(Al), respectively. The elevated TL values at 100 Hz for MIL-53(Al) and FeBTC were more prominent compared to the other MOFs tested. This low-frequency range with elevated TL may be the stiffness-controlled region, before the onset of the first resonance of the MOF disc.3 Importantly, the different pore sizes and topologies of the studied MOFs result in unique resonances, so there is potential to tailor the MOF composition and structure for a frequency range of interest. FeBTC was demonstrated to be the most effective unmodified absorptive material, as it’s outperformance of mass law was greatest relative to the other MOFs tested (Figure 2a). Although

ACS Paragon Plus Environment

Page 2 of 9

Page 3 of 9 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60


Figure 2. Panel A shows the normal incidence sound transmission loss (TL) measurements conducted on 100 mm unmodified MOF discs with resonances in the 160-315 Hz range. The mass-law predictions are plotted as solid curves with colors that correspond to the experimental plots. Panel B shows the experimental and calculated TL (please note the different scales) of silica and basaltic rock discs. The uncertainties for TL are smaller than the plotted points. Lastly, we measured the TL of the flexible MIL-53(Al) samples that had been modified with flexible glutarate and adipate linkers (Figure 3). The modified MIL-53(Al) samples also exhibited absorptive acoustic metamaterial properties, outperforming mass law for the entire 100-1250 Hz frequency range. The enhanced flexibility of the frameworks resulted in greater transmission loss for both MIL-53(Al)-GA and MIL-53(Al)-AA relative to mass law predictions, with MIL-53(Al)-AA exhibiting the most pronounced enhancement (Figure 3). In fact, MIL-53(Al)-AA outperformed mass law to a greater extent than unmodified FeBTC. New dips in TL at 160 Hz, not apparent for MIL-53(Al), for both MIL-53(Al)GA and MIL-53(Al)-AA were observed, strongly suggestive of new resonances attributable to the flexible linkers. The corresponding new local TL maxima were detected at 200 and 250 Hz for MIL-53(Al)-GA and MIL-53(Al)-AA, respectively. The TL behavior of MIL-53(Al)-AA retained the original MIL-53(Al) dip at 315 Hz, but the resonance local minima for MIL-53(Al)-GA shifted to ~275 Hz. This shift is suggestive of radiative acoustic feedback, which may occur when resonating materials have multiple flexible components.30 The results likely indicate that the MIL-53(Al) samples exhibit reversible structural transitions that depend on the nature and magnitude of absorbed acoustic waves. The modification of framework flexibility for acoustic metamaterials also allows for tunable manipulation of acoustic properties. Mixtures of different MOF structures, compositions, and flexible components could lead to broadband attenuation and increase the number of detectable, diagnostic, and tunable resonances. In summary, we have developed and tested the usefulness of prototypical and modified MOFs for low-frequency sound attenuation and contrast agent applications. We demonstrated that HKUST-1, FeBTC, and three variations of flexible MIL-53(Al) are absorptive acoustic metamaterials which outperform mass law predictions of sound transmission loss behaviour. To the best of our knowledge, these results represent first example on MOF based acoustic metamaterials for low-frequency applications. These lowfrequency properties are tunable, as they depend on the topology and flexibility of the MOF. These lightweight and dispersible metamaterials may be used to as additives for construction

materials with superior sound adsorption. MOF-based insulators

Figure 3. Normal incidence sound transmission loss (TL) measurements conducted on MIL-53(Al) discs that were unmodified or substituted with flexible glutaric acid (GA) or adipic acid (AA) linkers and compared with predicted TL according to mass law. The uncertainties for TL are smaller than the plotted points. will be thin and lightweight, ideal for use in buildings and transport craft (i.e. automobiles, spacecraft, airplanes, helicopters) with size, mass, and/or fuel efficiency restrictions. Addition of acoustic metamaterial MOFs to these materials may also have beneficial secondary properties, including air purification and anti-mold properties. Acoustic metamaterial MOFs may also be a disruptive breakthrough for subsurface geophysical monitoring and mapping, including tracking injected MOF-bearing fluids. Integrating acoustic MOFs into borehole cements may also enable noninvasive monitoring of cement stability and wellbore integrity. We


ACS Applied Materials & Interfaces 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

are currently working on identifying more MOF candidates for acoustic applications and designing hybrid MOF-based acoustically responsive materials. We are also developing waterstable acoustic MOF contrast agent nanoparticles for injection into bench-scale geophysical experiments and field demonstrations. ASSOCIATED CONTENT Supporting Information The Supporting Information is available free of charge on the ACS Publications website. Methods section detailing MOF preparation, disc preparation, acoustic impedance tube methods, and Xray diffraction (XRD) characterization methods; XRD results for MOF samples, both before and after hydraulic pressing AUTHOR INFORMATION

Corresponding Author * Corresponding Author Q.R.S. Miller, [email protected]

Present Addresses †Present address of KWJ is Knowles Intelligent Audio, 331 Fairchild Dr., Mountain View, CA 94043, United States

Author Contributions This manuscript was written through contributions of all authors. All authors have given final approval to the final version of the manuscript.

ORCID Quin R.S. Miller Satish K. Nune H. Todd Schaef Ki Won Jung

0000-0003-3009-9702 0000-0002-2971-0554 0000-0002-4546-3979 0000-0001-9847-3532

Notes The authors declare no competing financial interests. ACKNOWLEDGMENT This material is based upon work supported by the U.S. Department of Energy Office of Fossil Energy (DOE FE) at PNNL through the National Energy Technology Laboratory, Morgantown, West Virginia. We would also like to thank the CertainTeed Corporation for funding a precursor to the DOE FE project. We also thank Associate Editor Prof. Omar Farha and two anonymous reviewers, whose comments and feedback helped improve the manuscript. REFERENCES (1) Yang, Z.; Dai, H.; Chan, N.; Ma, G.; Sheng, P. Acoustic Metamaterial Panels for Sound Attenuation in the 50–1000 Hz Regime. Appl. Phys. Lett. 2010, 96 (4), 041906. (2) Sharp, B. H. A Study of Techniques to Increase the Sound Insulation of Building Elements, US Department of Commerce, National Technical Information Service (NTIS): 1973. (3) Bies, D. A.; Hansen, C. H. Engineering Noise Control: Theory and Practice, Fourth Edition, Taylor & Francis: 2009. (4) Ohiri, K. A.; Evans, B. A.; Shields IV, C. W.; Gutiérrez, R. A.; Carroll, N. J.; Yellen, B. B.; López, G. P. Magnetically Responsive Negative Acoustic Contrast Microparticles for

Bioanalytical Applications. ACS Appl. Mater. Interfaces 2016, 8 (38), 25030-25035. (5) Winthaegen, P.; Arts, R.; Schroot, B. Monitoring Subsurface CO2 Storage. Oil & Gas Science and Technology-Revue D Ifp Energies Nouvelles 2005, 60 (3), 573-582, DOI: 10.2516/ogst:2005040. (6) McGrail, B. P.; Schaef, H. T.; Spane, F. A.; Cliff, J. B.; Qafoku, O.; Horner, J. A.; Thompson, C. J.; Owen, A. T.; Sullivan, C. E. Field Validation of Supercritical CO2 Reactivity with Basalts. Environ. Sci. & Technol. Lett. 2017, 4 (1), 6-10, DOI: 10.1021/acs.estlett.6b00387. (7) Schaef, H. T.; Davidson, C. L.; Owen, A. T.; Miller, Q. R. S.; Loring, J. S.; Thompson, C. J.; Bacon, D. H.; Glezakou, V. A.; McGrail, B. P. CO2 Utilization and Storage in Shale Gas Reservoirs: Experimental Results and Economic Impacts. Energy Procedia 2014, 63, 7844-7851. (8) Palmer, C.; Sito, Z. Nitrogen and Carbon Dioxide Fracturing Fluids for the Stimulation of Unconventional Shale Plays. AGH Drilling, Oil, Gas 2013, 30 (1), 191-198. (9) Mikhaltsevitch, V.; Lebedev, M.; Gurevich, B. Measurements of the Elastic and Anelastic Properties of Sandstone Flooded with Supercritical CO2. Geophys. Prospect. 2014, 62 (6), 1266-1277. (10) Cummer, S. A.; Christensen, J.; Alù, A. Controlling Sound with Acoustic Metamaterials. Nat. Rev. Mater. 2016, 1, 16001. (11) Yang, Z.; Mei, J.; Yang, M.; Chan, N.; Sheng, P. Membrane-Type Acoustic Metamaterial with Negative Dynamic Mass. Phys. Rev. Lett. 2008, 101 (20), 204301. (12) Liu, Z.; Zhang, X.; Mao, Y.; Zhu, Y.; Yang, Z.; Chan, C. T.; Sheng, P. Locally Resonant Sonic Materials. Science 2000, 289 (5485), 1734-1736. (13) Naify, C. J.; Chang, C.-M.; McKnight, G.; Scheulen, F.; Nutt, S. Membrane-Type Metamaterials: Transmission Loss of Multi-Celled Arrays. J. Appl. Phys. 2011, 109 (10), 104902. (14) Oh, J.-H.; Kim, J.; Lee, H.; Kang, Y.; Oh, I.-K. Directionally Antagonistic Graphene Oxide-Polyurethane Hybrid Aerogel as a Sound Absorber. ACS Appl. Mater. Interfaces 2018, 10 (26), 22650-22660, DOI: 10.1021/acsami.8b06361. (15) Lau, H. C.; Yu, M.; Nguyen, Q. P. Nanotechnology for Oilfield Applications: Challenges and Impact. J. Pet. Sci. Eng. 2017, 157, 1160-1169. (16) Meek, S. T.; Greathouse, J. A.; Allendorf, M. D. Metal‐Organic Frameworks: A Rapidly Growing Class of Versatile Nanoporous Materials. Adv. Mater. 2011, 23 (2), 249-267. (17) Annapureddy, H. V.; Nune, S. K.; Motkuri, R. K.; McGrail, B. P.; Dang, L. X. A Combined Experimental and Computational Study on the Stability of Nanofluids Containing Metal Organic Frameworks. J. Phys. Chem. B. 2015, 119 (29), 8992-8999. (18) Hong, D. H.; Suh, M. P. Enhancing CO2 Separation Ability of a Metal–Organic Framework by Post‐Synthetic Ligand Exchange with Flexible Aliphatic Carboxylates. Chem. Eur. J. 2014, 20 (2), 426-434. (19) Nandasiri, M. I.; Jambovane, S. R.; McGrail, B. P.; Schaef, H. T.; Nune, S. K. Adsorption, Separation, and Catalytic Properties of Densified Metal-Organic Frameworks. Coord. Chem. Rev. 2016, 311, 38-52. (20) Sun, Y.; Li, Y.; Tan, J.-C. Framework Flexibility of Zif-8 under Liquid Intrusion: Discovering Time-Dependent Mechanical Response and Structural Relaxation. PCCP 2018, 20 (15), 1010810113. (21) Yot, P. G.; Boudene, Z.; Macia, J.; Granier, D.; Vanduyfhuys, L.; Verstraelen, T.; Van Speybroeck, V.; Devic, T.; Serre, C.; Férey, G. Metal–Organic Frameworks as Potential Shock Absorbers: The Case of the Highly Flexible MIL-53 (Al). Chem. Commun. 2014, 50 (67), 9462-9464. (22) Su, Z.; Shaw, W. L.; Miao, Y.-R.; You, S.; Dlott, D. D.; Suslick, K. S. Shock Wave Chemistry in a Metal–Organic


Page 4 of 9

Page 5 of 9 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

ACS Applied Materials & Interfaces Framework. J. Am. Chem. Soc. 2017, 139 (13), 4619-4622, DOI: 10.1021/jacs.6b12956. (23) Lemoult, F.; Kaina, N.; Fink, M.; Lerosey, G. Wave Propagation Control at the Deep Subwavelength Scale In Metamaterials. Nat. Phys. 2012, 9, 55. (24) Boutin, A.; Coudert, F.-X.; Springuel-Huet, M.-A.; Neimark, A. V.; Férey, G.; Fuchs, A. H. The Behavior of Flexible Mil-53 (Al) Upon CH4 and CO2 Adsorption. J. Phys. Chem. C 2010, 114 (50), 22237-22244. (25) Hwang, I. H.; Bae, J. M.; Kim, W.-S.; Jo, Y. D.; Kim, C.; Kim, Y.; Kim, S.-J.; Huh, S. Bifunctional 3D Cu-MOFs Containing Glutarates and Bipyridyl Ligands: Selective CO2 Sorption and Heterogeneous Catalysis. Dalton Trans. 2012, 41 (41), 1275912765. (26) Reinsch, H.; Pillai, R. S.; Siegel, R.; Senker, J.; Lieb, A.; Maurin, G.; Stock, N. Structure and Properties of Al-MIL-53-Adp, a Breathing MOF Based on the Aliphatic Linker Molecule Adipic Acid. Dalton Trans. 2016, 45 (10), 4179-4186.

(27) ASTM, Standard Test Method for Measurement of Normal Incidence Sound Transmission of Acoustical Materials Based on the Transfer Matrix Method. West Conshohocken, PA, USA, 2009; Vol. E 2611-09. (28) Shahid, S.; Nijmeijer, K. High Pressure Gas Separation Performance of Mixed-Matrix Polymer Membranes Containing Mesoporous Fe(BTC). J. Membr. Sci. 2014, 459, 33-44, DOI: https://doi.org/10.1016/j.memsci.2014.02.009. (29) Kinsler, L. E.; Frey, A. R.; Coppens, A. B.; Sanders, J. V. Fundamentals of Acoustics, 4th Edition, John Wiley and Sons: New York, 2000. (30) Dosch, H. G. Radiative Feedback in Helmholtz Resonators with More than One Opening. J. Acoust. Soc. Am. 2016, 140 (5), 3576-3581, DOI: 10.1121/1.4966268.




Page 6 of 9

6

Page 7 of 9 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60


The top panel shows the schematic of the air-filled acoustic impedance tube setup, used to deter-mine normal incidence transmission loss. Photographs of the four unmodified metal-organic frame-work 100 mm discs that were tested are shown below the impedance tube. 125x71mm (220 x 220 DPI)



Panel A shows the normal incidence sound transmission loss (TL) measurements conducted on 100 mm unmodified MOF discs with reso-nances in the 160-315 Hz range. The mass-law predictions are plotted as solid curves with colors that correspond to the experimental plots. Panel B shows the experimental and calculated TL (please note the different scales) of silica and basaltic rock discs. The uncertainties for TL are smaller than the plotted points. 243x109mm (149 x 149 DPI)


Page 8 of 9

Page 9 of 9 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60


Normal incidence sound transmission loss (TL) measurements conducted on MIL-53(Al) discs that were unmodified or substituted with flexible glutaric acid (GA) or adipic acid (AA) linkers and compared with predicted TL according to mass law. The uncertainties for TL are smaller than the plotted points. 127x109mm (149 x 149 DPI)


Microporous and Flexible Framework Acoustic Metamaterials for

Recommend Documents