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Nanoporous Iron Oxide/Carbon Composites Through In-Situ Deposition of Prussian Blue Nanoparticles on Graphene Oxide Nanosheets A

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Nanoporous Iron Oxide/Carbon Composites Through In-Situ Deposition of Prussian Blue Nanoparticles on Graphene Oxide Nanosheets A nanomaterials Article Nanoporous Iron Oxide/Carbon Composites through In-Situ Deposition of Prussian Blue Nanoparticles on Graphene Oxide Nanosheets and Subsequent Thermal Treatment for Supercapacitor Applications 1, 2,3,4, , 1,5, 6, Alowasheeir Azhar y, Yusuke Yamauchi * y, Abeer Enaiet Allah y, Zeid A. Alothman * , Ahmad Yacine Badjah 6, Mu. Naushad 6 , Mohamed Habila 6, Saikh Wabaidur 6, Jie Wang 1,* and Mohamed Barakat Zakaria 1,3,7,* 1 International Center for Materials Nanoarchitectonics (WPI-MANA), National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan; [email protected] (A.A.); [email protected] (A.E.A.) 2 Key Laboratory of Eco-Chemical Engineering, College of Chemistry and Molecular Engineering, Qingdao University of Science and Technology, Qingdao 266042, China 3 School of Chemical Engineering and Australian Institute for Bioengineering and Nanotechnology (AIBN), The University of Queensland, Brisbane, QLD 4072, Australia 4 Department of Plant & Environmental New Resources, Kyung Hee University, 1732 Deogyeong-daero, Giheung-gu, Yongin-si, Gyeonggi-do 446-701, Korea 5 Chemistry Department, Faculty of Science, Beni-Suef University, Beni-Suef 62511, Egypt 6 Advanced Material Research Chair, Chemistry Department, College of Science, King Saud University, P.O. Box 2455, Riyadh 11451, Saudi Arabia; [email protected] (A.Y.B.); [email protected] (M.N.); [email protected] (M.H.); [email protected] (S.W.) 7 Department of Chemistry, Faculty of Science, Tanta University, Tanta, Gharbeya 31527, Egypt * Correspondence: [email protected] (Y.Y.); [email protected] (Z.A.A.); [email protected] (J.W.); [email protected] (M.B.Z.) These authors equally contributed to this work. y Received: 20 March 2019; Accepted: 8 May 2019; Published: 21 May 2019 Abstract: This work reports the successful preparation of nanoporous iron oxide/carbon composites through the in-situ growth of Prussian blue (PB) nanoparticles on the surface of graphene oxide (GO) nanosheets. The applied thermal treatment allows the conversion of PB nanoparticles into iron oxide (Fe2O3) nanoparticles. The resulting iron oxide/carbon composite exhibits higher specific capacitance at all scan rates than pure GO and Fe2O3 electrodes due to the synergistic contribution of electric double-layer capacitance from GO and pseudocapacitance from Fe2O3. Notably, even at 1 a high current density of 20 A g− , the iron oxide/carbon composite still shows a high capacitance retention of 51%, indicating that the hybrid structure provides a highly accessible path for diffusion of electrolyte ions. Keywords: nanoporous materials; iron oxide; carbon composites; Prussian blue; supercapacitors 1. Introduction Hybrid materials have been extensively studied for energy storage applications due to the possibility of combining the advantages of two (or more) individual constituents to meet the demand for recent technological applications [1,2]. In recent years, coordination polymers (CPs), especially Prussian Blue (PB) and its analogues (PBAs), have been widely used for energy storage applications because of their unique features, such as their open frameworks, high stability, and redox activity. Nanomaterials 2019, 9, 776; doi:10.3390/nano9050776 www.mdpi.com/journal/nanomaterials Nanomaterials 2019, 9, x FOR PEER REVIEW 2 of 11 applications because of their unique features, such as their open frameworks, high stability, and Nanomaterials 2019, 9, 776 2 of 11 redox activity. However, the poor conductivity of these materials presents a major obstacle for practical use. Hybrid materials composed of PB and rGO nanosheets have been investigated to some However,extent recently the poor [2–4]. conductivity of these materials presents a major obstacle for practical use. Hybrid materialsIn general, composed carbon-based of PB and materials rGO nanosheets [5], such have as graphene been investigated oxide (GO), to some reduced extent graphene recently [oxide2–4]. (rGO),In and general, carbon carbon-based nanotubes, materialsor conducting [5], such poly asmers, graphene such as oxide polypyrrole (GO), reduced (PPy) and graphene polyaniline oxide (rGO),(PANI), and are carbon typically nanotubes, used to orimprove conducting the conducti polymers,vity such of PB-based as polypyrrole materials (PPy) [6–10]. and polyanilineThe active (PANI),functional are groups typically on usedthe basal to improve planes theand conductivity edges of GO of nanoshee PB-basedts materialsallow for [6the–10 adsorption]. The active of functionalcations which groups act on as the nucleation basal planes centers and edgesfor the of gr GOowth nanosheets of PB nanoparticles, allow for the adsorption thus making of cations them whichattractive act asto nucleationbe hybridized centers with for PB. the In growth addition, of PB the nanoparticles, developed reduced thus making GO (rGO) them attractivenanosheets to beduring hybridized composites with synthesis PB. In addition, possess the high developed electrical reduced conductivity GO (rGO) and nanosheetsimproved structural during composites stability. synthesisOur group possess has reported high electrical the in-situ conductivity growth andof vari improvedous cyano-bridged structural stability. CPs on Our the group surface has of reported GO by thedifferent in-situ methods growth of[11]. various cyano-bridged CPs on the surface of GO by different methods [11]. PB and PBAs have been utilized as precursors for the preparation of metal oxides with good electrochemical performanceperformance for for energy energy storage storage applications applications by by means means of thermalof thermal decomposition decomposition [12]. In[12]. particular, In particular, iron oxides iron (Fe oxidesxOy) have(FexO showny) have some shown promise some as anpromise electrode as materialan electrode for supercapacitors material for owingsupercapacitors to their high owing theoretical to their high specific theoretical capacitance, specific cost-e capacitance,ffectiveness, cost-effectiveness, low toxicity, excellent low toxicity, safety, andexcellent wide safety, abundance and wide [13 ,14abundance]. In this [13,14]. work, In we this demonstrate work, we demonstrate the facile preparation the facile preparation of a PB/GO of compositea PB/GO composite through the through in-situ the deposition in-situ deposition of PB nanoparticles of PB nanoparticles on GO nanosheets on GO nanosheets and the subsequent and the thermalsubsequent treatment thermal to converttreatment the PBto/ GOconver compositet the toPB/GO nanoporous composite Fe2O 3to/carbon nanoporous composite Fe (Scheme2O3/carbon1). Thecomposite resulting (Scheme Fe2O3 /1)carbon. The compositeresulting Fe shows2O3/carbon high specificcomposite capacitance, shows high excellent specific rate capacitance, capability, andexcellent good rate cycling capability, stability and for good supercapacitors. cycling stability for supercapacitors. Scheme 1. 1. SchematicSchematic illustration illustration for the for preparation the preparation of the ofPrussian the Prussian blue/graphene blue/graphene oxide (PB/GO) oxide (PBcomposite/GO) composite and the subsequent and the subsequentthermal conversi thermalon to conversion nanoporous to iron nanoporous oxide/carbon iron (Fe oxide2O3/carbon)/carbon (Fecomposite.2O3/carbon) composite. 2. Experimental Section 2. Experimental Section 2.1. Chemicals 2.1. Chemicals Sodium ferrocyanide (II) decahydrate (Na4[Fe(CN)6] 10H2O) was purchased from Sigma-Aldrich, Sodium ferrocyanide (II) decahydrate (Na4[Fe(CN)· 6]·10H2O) was purchased from Co., St. Louis, MO, USA. The sulfuric acid solution was purchased from Nacalai tesque, Inc., Kyoto, Sigma-Aldrich, Co., St. Louis, MO, USA. The sulfuric acid solution was purchased from Nacalai Japan. Potassium hydroxide, sodium nitrate and iron (III) chloride hexahydrate (FeCl 6H O) were tesque, Inc., Kyoto, Japan. Potassium hydroxide, sodium nitrate and iron (III) chloride3 ·hexahydrate2 purchased from FUJIFILM Wako Pure Chemicals, Osaka, Japan. Nanographite platelets (N008-100-N) (FeCl3·6H2O) were purchased from FUJIFILM Wako Pure Chemicals, Osaka, Japan. Nanographite of 100 nm thickness were used as a raw material to prepare graphene oxide (GO) sheets (Angstron platelets (N008-100-N) of 100 nm thickness were used as a raw material to prepare graphene oxide materials, Dayton, OH, USA). Potassium permanganate (KMnO4) and hydrogen peroxide (H2O2) were (GO) sheets (Angstron materials, Dayton, OH, USA). Potassium permanganate (KMnO4) and purchased from Kanto Chemicals Co., Inc., Tokyo, Japan. All chemical reagents were used without hydrogen peroxide (H2O2) were purchased from Kanto Chemicals Co., Inc., Tokyo, Japan. All further purification. chemical reagents were used without further purification. 2.2. Synthesis of GO Nanosheets 2.2. Synthesis of GO Nanosheets GO nanosheets were prepared according to the modified Hummer’s method [1]. In a typical process, graphite powder (N008-100-N, carbon source) and sodium nitrate were mixed together and then a concentrated sulphuric acid solution (7.67 mL) was added into this suspension under constant Nanomaterials 2019, 9, x; doi: FOR PEER REVIEW www.mdpi.com/journal/nanomaterials stirring for 1 h. Subsequently, KMnO4 (1.0 g) was added into the resulting mixture solution while maintaining the temperature at lower than 20 ◦C. The reaction mixture was then stirred at 35 ◦C for 2 h Nanomaterials 2019, 9, 776 3 of 11 followed by the addition of pure water (83 mL) under
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