<?xml version="1.0" encoding="UTF-8"?><!DOCTYPE article  PUBLIC "-//NLM//DTD Journal Publishing DTD v3.0 20080202//EN" "http://dtd.nlm.nih.gov/publishing/3.0/journalpublishing3.dtd"><article xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink" dtd-version="3.0" xml:lang="en" article-type="research article"><front><journal-meta><journal-id journal-id-type="publisher-id">Graphene</journal-id><journal-title-group><journal-title>Graphene</journal-title></journal-title-group><issn pub-type="epub">2169-3439</issn><publisher><publisher-name>Scientific Research Publishing</publisher-name></publisher></journal-meta><article-meta><article-id pub-id-type="doi">10.4236/graphene.2017.63005</article-id><article-id pub-id-type="publisher-id">Graphene-76048</article-id><article-categories><subj-group subj-group-type="heading"><subject>Articles</subject></subj-group><subj-group subj-group-type="Discipline-v2"><subject>Chemistry&amp;Materials Science</subject></subj-group></article-categories><title-group><article-title>
 
 
  One-Step One Chemical Synthesis Process of Graphene from Rice Husk for Energy Storage Applications
 
</article-title></title-group><contrib-group><contrib contrib-type="author" xlink:type="simple"><name name-style="western"><surname>Pushpendra</surname><given-names>Singh</given-names></name><xref ref-type="aff" rid="aff1"><sup>1</sup></xref></contrib><contrib contrib-type="author" xlink:type="simple"><name name-style="western"><surname>Jitendra</surname><given-names>Bahadur</given-names></name><xref ref-type="aff" rid="aff1"><sup>1</sup></xref></contrib><contrib contrib-type="author" xlink:type="simple"><name name-style="western"><surname>Kaushik</surname><given-names>Pal</given-names></name><xref ref-type="aff" rid="aff2"><sup>2</sup></xref></contrib></contrib-group><aff id="aff1"><addr-line>Centre of Nanotechnology, Indian Institute of Technology, Roorkee, India</addr-line></aff><aff id="aff2"><addr-line>Department of Mechanical and Industrial Engineering, Indian Institute of Technology, Roorkee, India</addr-line></aff><pub-date pub-type="epub"><day>08</day><month>05</month><year>2017</year></pub-date><volume>06</volume><issue>03</issue><fpage>61</fpage><lpage>71</lpage><history><date date-type="received"><day>April</day>	<month>10,</month>	<year>2017</year></date><date date-type="rev-recd"><day>Accepted:</day>	<month>May</month>	<year>5,</year>	</date><date date-type="accepted"><day>May</day>	<month>8,</month>	<year>2017</year></date></history><permissions><copyright-statement>&#169; Copyright  2014 by authors and Scientific Research Publishing Inc. </copyright-statement><copyright-year>2014</copyright-year><license><license-p>This work is licensed under the Creative Commons Attribution International License (CC BY). http://creativecommons.org/licenses/by/4.0/</license-p></license></permissions><abstract><p>
 
 
  Few layer graphene was synthesized using rice husk ash (RHA) and potassium hydroxide (KOH). This methodology demonstrates the utility of RHA as carbon source for graphene synthesis and as a protective barrier against oxidation of parent rice husk and KOH mixture. Oxidation may occur during synthesis process due to high temperature annealing of RHA and KOH mixture. Electrochemical characterization showed decent capacitance value 86 F
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  . XRD and Raman spectroscopy analysis confirmed the presence of graphitic structure. Transmission electron microscopy visually confirmed presence of few layer graphene. Novelty of this synthesis technique can be described as one-pot, one chemical synthesis technique. Use of natural precursor makes this technique highly cost effective for large scale production.
 
</p></abstract><kwd-group><kwd>Rice Husk</kwd><kwd> Graphene</kwd><kwd> Silicon Dioxide</kwd><kwd> Cyclic Voltammetry</kwd></kwd-group></article-meta></front><sec id="s1"><title>1. Introduction</title><p>Graphene is a 2D carbon allotrope with honeycomb lattice structure. Individual carbon atoms are bonded by sp<sup>2</sup> hybridization [<xref ref-type="bibr" rid="scirp.76048-ref1">1</xref>] . Graphene has outstanding properties like: excellent electrical and thermal conductivity, flexibility, optical transparency, high specific surface area and much more. These properties make it suitable for various applications, like energy storage and harvesting application (super capacitors, battery, solar cell and so on) [<xref ref-type="bibr" rid="scirp.76048-ref2">2</xref>] - [<xref ref-type="bibr" rid="scirp.76048-ref7">7</xref>] , fabrication of transistors [<xref ref-type="bibr" rid="scirp.76048-ref8">8</xref>] [<xref ref-type="bibr" rid="scirp.76048-ref9">9</xref>] , biomedical application [<xref ref-type="bibr" rid="scirp.76048-ref10">10</xref>] [<xref ref-type="bibr" rid="scirp.76048-ref11">11</xref>] , designing mechanically robust materials [<xref ref-type="bibr" rid="scirp.76048-ref12">12</xref>] [<xref ref-type="bibr" rid="scirp.76048-ref13">13</xref>] [<xref ref-type="bibr" rid="scirp.76048-ref14">14</xref>] [<xref ref-type="bibr" rid="scirp.76048-ref15">15</xref>] etc.</p><p>Synthesis of single layer of graphite has been reported as early as in 1975 by B. Lang [<xref ref-type="bibr" rid="scirp.76048-ref16">16</xref>] . After some scattered attempts by various scientist, finally Novoselov et al. have gained the credit for discovery of graphene in 2004 [<xref ref-type="bibr" rid="scirp.76048-ref17">17</xref>] . They introduced a reproducible technique of graphene synthesis by mechanical exfoliation but this technique is not suitable for large scale production. There are some other well established methods also available for synthesis of graphene such as chemical vapour deposition, chemical reduction of graphene oxide and epitaxial growth on silicon carbide.</p><p>Currently, many researchers are trying to develop green synthesis methods for graphene production [<xref ref-type="bibr" rid="scirp.76048-ref18">18</xref>] [<xref ref-type="bibr" rid="scirp.76048-ref19">19</xref>] [<xref ref-type="bibr" rid="scirp.76048-ref20">20</xref>] . The purpose of green synthesis process is to use less toxic chemicals and natural precursor. Muramatsu et al. have reported synthesis of graphene from rice husk using KOH and carbon black [<xref ref-type="bibr" rid="scirp.76048-ref20">20</xref>] .</p><p>In this research work, we have successfully replaced carbon black by Rice husk itself, in this way, this approach become even more cost effective synthesis methodology. In our synthesis process we have used RHA as carbon source for graphene synthesis and KOH as activation agent. The obtained results have revealed successful synthesis of few layer graphene. Cyclic voltammetry has been performed to evaluate electrochemical performance for energy storage application.</p></sec><sec id="s2"><title>2. Materials and Methods</title><p>The synthesis process is shown in <xref ref-type="fig" rid="fig1">Figure 1</xref>, in typical synthesis process, analytical grade reagent KOH and rice husk were purchased from local market. In typical synthesis process, rice husk collected from local rice mill, was washed several times to remove silica and other contamination as much as possible. After washing, the RHA was prepared by the combustion of rice husk into air. Furthermore, 3 gm of rice husk ash was mixed with 15 gm of KOH and followed by grinding process for 15 min. The mixture of rice husk and KOH was compacted into porcelain crucible. This crucible was covered with ceramic wool and fixed into a larger graphite crucible. The top of the graphite crucible was covered</p><fig id="fig1"  position="float"><label><xref ref-type="fig" rid="fig1">Figure 1</xref></label><caption><title> Experimental set-up for synthesis of RHA derived graphene</title></caption><graphic mimetype="image"   position="float"  xlink:type="simple"  xlink:href="http://html.scirp.org/file/1-2690102x2.png"/></fig><p>with sufficient amount of sacrificial RHA to provide a barrier against oxidation of the sample inside porcelain crucible. This sample was annealed at 900˚C for 2 hours in muffle furnace. After this activation treatment, sample was washed several times with distilled water to remove excess KOH and dried at 100˚C for 24 hours.</p><p>Synthesized material was characterized by Field emission scanning electron microscopy (FESEM) Zeiss-Ultra Plus, Gemini Co. Transmission Electron Microscopy (TEM) images were obtained using TECNAI G2 20 S-TWIN (FEI Netherlands), X-ray diffraction (XRD) study was done by Bruker AXS Diffractometer D8, Thermal analysis of the synthesized sample was done using Thermogravimetric analysis (TGA) SII 6300 Exstar Instrument from 0 to 820˚C at constant scanning rate of 10˚C/min; Fourier transform infrared spectroscopy (FTIR) by Perkin Elmer, Raman spectroscopy by InviaRenishaw Raman spectrophotometer with Excitation Wavelength of 514 nm Argon ion laser were done. Cyclic voltammetry has been used for electrochemical analysis of the specimen using Basi EC epsilon-EClipse.</p></sec><sec id="s3"><title>3. Results and Discussion</title></sec><p>The FESEM images of successfully synthesized Graphene by activation treatment of RHA using KOH are shown in <xref ref-type="fig" rid="fig2">Figure 2</xref>. From this morphological analysis, flakes of graphene sheets with silica nanoparticles can be observed clearly. Herein, the dual function of KOH is; removal of amorphous carbon and separation of individual graphene sheet by intercalation of potassium atoms.</p><p>TEM images of RHA derived graphene by KOH activation are shown in above <xref ref-type="fig" rid="fig3">Figure 3</xref>. The micro graphical images have confirmed the synthesis of few layer graphene. From these images, we can observe the few layer graphene and agglomeration of silica particles. In the inset, selected area electron diffraction pattern (SAED) has shown, the individual spots have merged into the rings. This shows the characteristic of polycrystalline sample [<xref ref-type="bibr" rid="scirp.76048-ref21">21</xref>] and suggests the stacking of graphene sheets and aggregation of silica particles with random arrangement.</p><p>FTIR spectrum of rice husk derived graphene-silica composite is shown in <xref ref-type="fig" rid="fig4">Figure 4</xref>. From FTIR spectra, the adsorption band at 1040 cm<sup>−1</sup> and 660 cm<sup>−1 </sup>which reflect asymmetric and symmetric stretches of Si-O-Si, respectively [<xref ref-type="bibr" rid="scirp.76048-ref22">22</xref>] . Moreover, the absorption band at 1420 cm<sup>−1</sup> has been observed due to the Si-O-C=O bonding [<xref ref-type="bibr" rid="scirp.76048-ref23">23</xref>] and the peak at 1600 cm<sup>−1</sup> in the spectrum confirms the presence of aromatic -C=C- bond [<xref ref-type="bibr" rid="scirp.76048-ref24">24</xref>] . The infrared band at 3000-3500 cm<sup>−1</sup> appears due to the asymmetric stretching and bending vibration of surface hydroxyls and adsorbed water [<xref ref-type="bibr" rid="scirp.76048-ref25">25</xref>] .</p><p>XRD pattern of prepared graphene by the activating of RHA using KOH at 900˚C is shown in <xref ref-type="fig" rid="fig5">Figure 5</xref>. From XRD analysis, the diffraction peaks around 20.96˚, 45.66˚ have been assigned with lattice plane (111) of cristobalite silica (JCPDS card No.: 89-3435) and (100) corresponds to graphitic structure of carbon, the weak intense peaks (100) of graphene specifies the non-appearance of a repeatedly stacked graphitic structure [<xref ref-type="bibr" rid="scirp.76048-ref20">20</xref>] .</p><back><ref-list><title>References</title><ref id="scirp.76048-ref1"><label>1</label><mixed-citation publication-type="other" xlink:type="simple">Novoselov, K.S., Falko, V.I., Colombo, L., Gellert, P.R., Schwab, M.G. and Kim, K. (2012) A Roadmap for Graphene. Nature, 490, 192-200. https://doi.org/10.1038/nature11458</mixed-citation></ref><ref id="scirp.76048-ref2"><label>2</label><mixed-citation publication-type="other" xlink:type="simple">Tan, Y.B. and Lee, J.M. (2013) Graphene for Supercapacitor Applications. 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