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In Situ Production of Graphene-Fiber Hybrid Structures Mandana Akia, Lee Daniel Cremar, Mircea Chipara, Edgar Munoz, Hilario Cortez, Hector de Santiago, Fernando J. Rodriguez-Macias, Yadira I. Vega-Cantú, Hamidreza Arandiyan, Hongyu Sun, Timothy P. Lodge, Yuanbing Mao, and Karen Lozano ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.7b07509 • Publication Date (Web): 12 Jul 2017 Downloaded from http://pubs.acs.org on July 13, 2017
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ACS Applied Materials & Interfaces
In Situ Production of Graphene-Fiber Hybrid Structures
Mandana Akia1, Lee Cremar1, Mircea Chipara2, Edgar Munoz1, Hilario Cortez1, Hector de Santiago3, Fernando J. Rodriguez-Macias4,5, Yadira I. Vega-Cantú4,5, Hamidreza Arandiyan6, Hongyu Sun7, Timothy P. Lodge8, Yuanbing Mao3, Karen Lozano1*
1
Department of Mechanical Engineering, University of Texas Rio Grande Valley, 1201 West University Drive, Edinburg, Texas 78539, United States
[email protected],
[email protected],
[email protected],
[email protected],
[email protected] 2
Department of Physics, University of Texas Rio Grande Valley, 1201 West University Drive, Edinburg, Texas, 78539, United States
[email protected] 3
Department of Chemistry, University of Texas Rio Grande Valley, 1201 West University Drive, Edinburg, Texas, 78539, United States
[email protected],
[email protected] 4
Tecnologico de Monterrey, Campus Monterrey, Ave. Eugenio Garza Sada 2501, Monterrey, N.L., México, 64849
[email protected],
[email protected] 5
Universidade Federal de Pernambuco, Pós-Graduação em Ciência de Materiais, Avenida Jornalista Aníbal Fernandes, Recife, PE, Brasil, 50740-560. 6
Particles and Catalysis Research Group, School of Chemical Engineering, The University of New South Wales, Sydney, New South Wales 2052, Australia
[email protected] 7
Department of Micro- and Nanotechnology, Technical University of Denmark, 2800 Kongens, Lyngby, Denmark
[email protected] 8
Department of Chemistry and Department of Chemical Engineering & Materials Science, University of Minnesota, Minneapolis, MN 55455, United States
[email protected] Corresponding author: Professor Karen Lozano at
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Abstract We report a scalable method to obtain a new material where large graphene sheets form webs linking carbon fibers. Film-fiber hybrid nonwoven mats are formed during fiber processing and converted to carbon structures after a simple thermal treatment. This contrasts with multi-step methods that attempt to mix previously prepared graphene and fibers, or require complicated and costly processes for deposition of graphene over carbon fibers. The developed graphene-fiber hybrid structures have seamless connections between graphene and fibers, and in fact the graphene “veils” extend directly from one fiber into another forming a continuous surface. The graphene-fiber hybrid structures are produced in situ from aqueous poly(vinyl alcohol) solutions. The solutions were subjected to centrifugal spinning to produce fine nanofiber mats. The addition of salt to the polymer solution stimulated a capillarity effect that promoted the formation of thin veils, which become graphene sheets upon dehydration by sulfuric acid vapor followed by carbonization (at relatively low temperatures, below 800 °C). These veils extend over several micrometers within the pores of the fiber network, and consist of crystalline graphene layers that crosslink the fibers to form a highly interconnected hybrid network. The surface area and pore diameter of the hybrid structures were measured to be 521 m2g–1 and 10 nm, respectively. The resulting structure shows high electrical conductivity, 550 S/m, and promising shielding of electromagnetic interference, making it an attractive system for a broad range of electronic applications.
Keywords: aqueous salt-polymer solutions; centrifugal spinning; nanofibers; carbonization; graphene; fabrication
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ACS Applied Materials & Interfaces
1 Introduction Graphene-fiber hybrid structures (GFHS) with homogeneous dispersion and optimal interfaces between fibers and graphene sheets are rapidly gaining attention given the potential practical applications in a wide range of electronic devices1. Major obstacles in the fabrication of GFHS include graphene availability, the cost of precursors, multistep and time consuming processes, difficulties in mixing, and agglomeration of graphene sheets due to strong interlayer attractions, which leads to a reduction in specific surface area2-4. Some studies have overcome the agglomeration issue by chemical functionalization (e.g., by installation of functional groups, which break the sp2 bonding that gives graphene many of its properties) or insertion of lower dimensional nanostructures as spacers, further increasing needed materials and processing steps58
. Reports have demonstrated that the surface area of the developed GFHS is strongly affected by
the size of the selected fiber system. Hybrid systems of graphene embedded in cotton fibers with fiber diameters in a range of 5-10 µm have shown high surface area, 450 m2 g-1 9. Other studies on graphene hybrid systems with fiber diameters between 25-110 µm have reported high surface area, up to 400 m2 g-1 4,10,11.
This work demonstrates for the first time a facile, cost effective and scalable process to grow GFHS in situ. The developed process overcomes major hurdles for scaling up, potentially unleashing the foreseen commercial growth of GFHS for use in multifunctional composites, sensors, filtration, and electronic applications. Figure 1 shows a schematic representation of this unique production method, which presents important economic and environmental advantages for large-scale GFHS production.
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Figure 1. (a) An aqueous solution of sodium chloride and polyvinyl alcohol (PVA) is subjected to Forcespinning, a process that uses centrifugal forces to drive the material through a designed set of orifices within a spinneret, producing nonwoven fine fiber mats. This method can produce hundreds of meters per minute with control of areal density (g/m2). The prepared mats are then subjected to a sulfuric acid vapor dehydration process, followed by washing and low temperature carbonization (
