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Functional Graphene Nanomesh Foam† Energy & Environmental Science View Article Online COMMUNICATION View Journal | View Issue Functional graphene nanomesh foam† Yang Zhao,a Chuangang Hu,a Long Song,a Lixia Wang,a Gaoquan Shi,b Liming Daic Cite this: Energy Environ. Sci.,2014,7, a 1913 and Liangti Qu* Received 11th January 2014 Accepted 1st April 2014 DOI: 10.1039/c4ee00106k www.rsc.org/ees Rationally designed graphene nanomesh assembled foam (GMF) with hierarchical pore arrangement has been successfully fabricated for the Broader context fi rst time by a site-localized nanoparticle-induced etching strategy on Graphene nanomeshes (GNMs) with nanoscale periodic or quasi-periodic the basis of hydrothermally self-assembled graphene architecture. nanoholes having more active sites and edges are attracting extensive The newly developed GMF provides a new material platform for attention due to their open energy band gaps, enlarged specic surface developing high-performance functional devices. Specially, the N- areas, and high optical transmittances useful for applications in semi- conducting devices, photocatalysis, sensors and energy-related systems. and S-codoped GMF electrode exhibits excellent electrocatalytic However, the well-organized assembly of GNMs into multidimensional activities for oxygen reduction reaction (ORR), better than most of the architectures has been absent so far, although the rational arrangement of graphene-based ORR catalysts reported previously. individual graphene sheets into macroscopic architectures is essential for converting the remarkable microscopic characteristics of graphenes into macroscopic properties and functions. In this work, we report the Graphene nanomeshes (GNMs), a new class of fascinating gra- successful assembly of graphene nanomeshes into the structure-hierar- phene materials, have attracted extensive attention due to their chical foams (GMFs) for the rst time, in which the macroporous gra- open energy band gaps,1 enlarged specic surface areas, and phene network is composed of graphene sheets with in-plane nanopores. For this purpose, a site-localized nanoparticle-induced etching strategy high optical transmittances2 useful for applications in semi- 1 2c 3 has been newly developed on the basis of hydrothermally self-assembled conducting devices, photocatalysis, sensors and energy- graphene architecture. With hierarchical pore arrangement, favorable 4 related systems. Compared to the basal planes in normal gra- mass transport and the richly available graphene edges, the as-prepared phene sheets, the nanoscale periodic or quasi-periodic nano- GMF provides a new platform for developing high-performance functional Published on 01 April 2014. Downloaded by CASE WESTERN RESERVE UNIVERSITY 21/04/2015 17:37:26. holes within GNMs possess more active sites and edges for materials and devices. As demonstrated in this study, the N- and S-codo- ped GMF electrode exhibited excellent electrocatalytic activities for oxygen faster electron transport and higher electrocatalytic activity.5 reduction reaction, which is one of the best among all the graphene-based To date, graphene meshes are mainly produced by means of oxygen reduction catalysts reported previously. block copolymer lithography, plasma etching, photocatalytic oxidation and chemical vapor deposition,1,6 which are oen costly and tedious. Although solution oxidation methods2a,b characteristics of graphenes into macroscopic properties of 7 have been reported recently, however, there has been no practical signi cance. Among them, three-dimensional (3D)- achievement so far on well-organized assembly of GNMs into assembled graphene foams or networks are of particular multidimensional architectures. As is well known, the rational interest due to their tunable con guration, high porosity, large 8 arrangement of individual graphene sheets into specic archi- surface area and multi-path electron transport. Therefore, tectures is essential for converting the remarkable microscopic GNMs as building blocks for construction of large-scale 3D frameworks with hierarchical pore distributions provide a unique platform for design and development of novel graphene aKey Laboratory of Cluster Science, Ministry of Education of China, Beijing Key materials with desirable electrical conductivity, mechanical Laboratory of Photoelectronic/Electrophotonic Conversion Materials, Department of Chemistry, School of Science, Beijing Institute of Technology, Beijing 100081, P. R. stability, and edge activity for various new practical China. E-mail: [email protected] applications. bDepartment of Chemistry, Tsinghua University, Beijing 100084, P. R. China Herein, we report a rational approach for graphene mesh cDepartment of Macromolecular Science and Engineering, Case School of Engineering, assembled foams (GMFs), in which the macroporous graphene Case Western Reserve University, 10900 Euclid Avenue, Cleveland, Ohio 44106, USA network is composed of graphene sheets with in-plane nano- † Electronic supplementary information (ESI) available: The experimental details pores. In view of the fact that heteroatom-doping of graphene for preparation of GMF and other comparable catalysts, characterization, and ff additional results and discussion. See DOI: 10.1039/c4ee00106k could e ectively modulate its electronic characteristics, surface This journal is © The Royal Society of Chemistry 2014 Energy Environ. Sci.,2014,7,1913–1918 | 1913 View Article Online Energy & Environmental Science Communication and local chemical features essential for novel functions and device applications,9 we introduced a pyrrole (Py) monomer into GMFs for in situ polymerization to provide the N source and to prevent possible self-stacking of GNMs7c for mechanically stable and electrically conductive 3D GMFs with highly exposed holey graphene surfaces. With favorable mass transport through the hierarchically arranged pores, abundant edge active sites, and heteroatom-doping-induced electronic modulation, the resul- tant GMFs stand for a new type of functional materials that could greatly benet the high-performance energy-related devices. As an example demonstrated in this study, the nitrogen and sulfur co-doped GMF exhibited excellent electrocatalytic activity for ORR better than most of the graphene-based cata- lysts reported so far. The process for the fabrication of N-doped GMF (N-GMF) is illustrated in Fig. 1. We rst produced 3D graphene gel by hydrothermal treatment of homogeneous graphene oxide (GO) À dispersion (1 mg mL 1) with a 3 vol% Py monomer in a Teon- lined autoclave (Fig. 1a and b). The as-obtained gel was then immersed into an aqueous solution of FeCl3 to form a poly- pyrrole/graphene composite with encapsulated FeCl3 residues (Fig. S1†). At a high temperature (850 C), N atoms were doped into the graphene structure through decomposition of poly- 10a pyrrole (PPy). Meanwhile, the remaining FeCl3 within the foam was converted into Fe2O3 nanoparticles on graphene sheets (Fig. S2a–c†), which could locally etch the graphene basal planes10b to form holey GNMs (Fig. S2d & e†). Thus, GMFs were produced by the in situ Fe2O3 nanoparticle formation and etching during thermal treatment (Fig. 1). The formation of graphene meshes with uniform and high- Fig. 2 (a) Photograph and (b) scanning electron microscopy (SEM) density nanoholes (Figs 1c and 2) is dependent on the applied image of N-GMF. (c) SEM and (d) scanning transmission electron temperature and treatment time (Fig. S3a & b†). Aer etching microscopy (STEM) image of individual sheet within N-GMF. The inset for 2 h at above 800 C, many nanoholes appeared around Fe O in (d) is the enlarged TEM image of a single nanohole. (e) STEM image 2 3 and C-, N- and O-elemental mappings for a nanohole region of N- GMF. (f) XPS spectrum of N-GMF and (g) the corresponding high- resolution N 1s peak. Scale bars: (b) 10 mm; (c) 100 nm; (d) 500 nm (inset, 10 nm); (e) 50 nm. Published on 01 April 2014. Downloaded by CASE WESTERN RESERVE UNIVERSITY 21/04/2015 17:37:26. nanoparticles on the graphene planes (Fig. S2d & e†). Further increase in the treatment time and temperature led to the formation of large holes with irregular shapes (Fig. S3c & d†). These results indicate that graphene meshes can be effectively produced by the localized interface etching between Fe2O3 nanoparticles and graphene sheets at appropriate temperatures (Fig. 1c). A er removing Fe2O3 nanoparticles by HCl, N-GMF is obtained nally (Fig. 1d). The as-prepared N-GMF exhibited a 3D graphene framework with a porous structure (Fig. 2a and b). High resolution SEM and STEM images (Fig. 2c and d) clearly show the mesh struc- ture of N-GMF with a uniform pore size of ca. 2–50 nm, high nanohole density (about 5.0 Â 109 holes per cm2), and an inter- pore distance in the range of several nanometers to ca. 100 nm. A typical hole-structure is shown in the inset of Fig. 2d. The Brunauer–Emmett–Teller (BET) nitrogen adsorption isotherm Fig. 1 The fabrication process of N-GMF. (a) Py monomer dispersed in 2 À1 a GO suspension. (b) 3D Py/G obtained after hydrothermal treatment. revealed a speci c surface area of 362 m g (Fig. S4a and Table † 2 (c) N-GMF with intercalated Fe2O3 nanoparticles. (d) N-GMF after S1 ), much higher than that of common graphene foam (166 m À À being washed with HCl. g 1).10c The porosity of N-GMF (with a density of 4.5 mg cm 3) 1914 | Energy Environ. Sci.,2014,7,1913–1918 This journal is © The Royal Society of Chemistry 2014 View Article Online Communication Energy & Environmental Science is about 99.79% and the pore-size
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