Electro-Exfoliation of Graphite to Graphene in an Aqueous Solution of Inorganic Salt and the Stabilization of Its Sponge Structure with Poly(Furfuryl Alcohol)

We demonstrate an accessible and effective technique for exfoliating graphite foil and graphite powder into graphene in a water solution of inorganic salt. In our research, we report an electrochemical cathodic exfoliation in an aqueous solution of Na<sub>2</sub>SO<sub>4</sub>...

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Main Authors: Anna Ilnicka, Malgorzata Skorupska, Piotr Kamedulski, Jerzy P. Lukaszewicz
Format: Article
Language:English
Published: MDPI AG 2019-07-01
Series:Nanomaterials
Subjects:
Online Access:https://www.mdpi.com/2079-4991/9/7/971
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author Anna Ilnicka
Malgorzata Skorupska
Piotr Kamedulski
Jerzy P. Lukaszewicz
author_facet Anna Ilnicka
Malgorzata Skorupska
Piotr Kamedulski
Jerzy P. Lukaszewicz
author_sort Anna Ilnicka
collection DOAJ
description We demonstrate an accessible and effective technique for exfoliating graphite foil and graphite powder into graphene in a water solution of inorganic salt. In our research, we report an electrochemical cathodic exfoliation in an aqueous solution of Na<sub>2</sub>SO<sub>4</sub>. After electro-exfoliation, the resulting graphene was premixed with furfuryl alcohol (FA) and an inorganic template (CaCO<sub>3</sub> and Na<sub>2</sub>CO<sub>3</sub>). Once FA was polymerized to poly(furfuryl alcohol) (PFA), the mixture was carbonized. Carbon bridges originating in thermally-decomposed PFA joined exfoliated graphene flakes and stabilized the whole sponge-type structure after the nano-template was removed. Gases evolved at the graphite electrode (cathode) played an important role in the process of graphene-flake splitting and accelerated the change of graphite into graphene flakes. Starting graphite materials and graphene sponges were characterized using Raman spectroscopy, SEM, high-resolution transmission electron microscopy (HRTEM), elemental analysis, and low-temperature adsorption of nitrogen to determine their structure, morphology, and chemical composition. The discovered manufacturing protocol had a positive influence on the specific surface area and porosity of the sponges. The SEM and HRTEM studies confirmed a high separation degree of graphite and different agglomeration pathways. Raman spectra were analyzed with particular focus on the intensities of I<sub>D</sub> and I<sub>G</sub> peaks; the graphene-type nature of the sponges was confirmed.
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spelling doaj.art-6744e2d6b79b4b3781bb7c6254d131062022-12-22T00:01:29ZengMDPI AGNanomaterials2079-49912019-07-019797110.3390/nano9070971nano9070971Electro-Exfoliation of Graphite to Graphene in an Aqueous Solution of Inorganic Salt and the Stabilization of Its Sponge Structure with Poly(Furfuryl Alcohol)Anna Ilnicka0Malgorzata Skorupska1Piotr Kamedulski2Jerzy P. Lukaszewicz3Faculty of Chemistry, Nicolaus Copernicus University, Gagarina 7, 87-100 Torun, PolandFaculty of Chemistry, Nicolaus Copernicus University, Gagarina 7, 87-100 Torun, PolandFaculty of Chemistry, Nicolaus Copernicus University, Gagarina 7, 87-100 Torun, PolandFaculty of Chemistry, Nicolaus Copernicus University, Gagarina 7, 87-100 Torun, PolandWe demonstrate an accessible and effective technique for exfoliating graphite foil and graphite powder into graphene in a water solution of inorganic salt. In our research, we report an electrochemical cathodic exfoliation in an aqueous solution of Na<sub>2</sub>SO<sub>4</sub>. After electro-exfoliation, the resulting graphene was premixed with furfuryl alcohol (FA) and an inorganic template (CaCO<sub>3</sub> and Na<sub>2</sub>CO<sub>3</sub>). Once FA was polymerized to poly(furfuryl alcohol) (PFA), the mixture was carbonized. Carbon bridges originating in thermally-decomposed PFA joined exfoliated graphene flakes and stabilized the whole sponge-type structure after the nano-template was removed. Gases evolved at the graphite electrode (cathode) played an important role in the process of graphene-flake splitting and accelerated the change of graphite into graphene flakes. Starting graphite materials and graphene sponges were characterized using Raman spectroscopy, SEM, high-resolution transmission electron microscopy (HRTEM), elemental analysis, and low-temperature adsorption of nitrogen to determine their structure, morphology, and chemical composition. The discovered manufacturing protocol had a positive influence on the specific surface area and porosity of the sponges. The SEM and HRTEM studies confirmed a high separation degree of graphite and different agglomeration pathways. Raman spectra were analyzed with particular focus on the intensities of I<sub>D</sub> and I<sub>G</sub> peaks; the graphene-type nature of the sponges was confirmed.https://www.mdpi.com/2079-4991/9/7/971grapheneelectrochemical exfoliationaqueous solutionpoly(furfuryl alcohol)Raman spectroscopygraphite electrode
spellingShingle Anna Ilnicka
Malgorzata Skorupska
Piotr Kamedulski
Jerzy P. Lukaszewicz
Electro-Exfoliation of Graphite to Graphene in an Aqueous Solution of Inorganic Salt and the Stabilization of Its Sponge Structure with Poly(Furfuryl Alcohol)
Nanomaterials
graphene
electrochemical exfoliation
aqueous solution
poly(furfuryl alcohol)
Raman spectroscopy
graphite electrode
title Electro-Exfoliation of Graphite to Graphene in an Aqueous Solution of Inorganic Salt and the Stabilization of Its Sponge Structure with Poly(Furfuryl Alcohol)
title_full Electro-Exfoliation of Graphite to Graphene in an Aqueous Solution of Inorganic Salt and the Stabilization of Its Sponge Structure with Poly(Furfuryl Alcohol)
title_fullStr Electro-Exfoliation of Graphite to Graphene in an Aqueous Solution of Inorganic Salt and the Stabilization of Its Sponge Structure with Poly(Furfuryl Alcohol)
title_full_unstemmed Electro-Exfoliation of Graphite to Graphene in an Aqueous Solution of Inorganic Salt and the Stabilization of Its Sponge Structure with Poly(Furfuryl Alcohol)
title_short Electro-Exfoliation of Graphite to Graphene in an Aqueous Solution of Inorganic Salt and the Stabilization of Its Sponge Structure with Poly(Furfuryl Alcohol)
title_sort electro exfoliation of graphite to graphene in an aqueous solution of inorganic salt and the stabilization of its sponge structure with poly furfuryl alcohol
topic graphene
electrochemical exfoliation
aqueous solution
poly(furfuryl alcohol)
Raman spectroscopy
graphite electrode
url https://www.mdpi.com/2079-4991/9/7/971
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AT malgorzataskorupska electroexfoliationofgraphitetographeneinanaqueoussolutionofinorganicsaltandthestabilizationofitsspongestructurewithpolyfurfurylalcohol
AT piotrkamedulski electroexfoliationofgraphitetographeneinanaqueoussolutionofinorganicsaltandthestabilizationofitsspongestructurewithpolyfurfurylalcohol
AT jerzyplukaszewicz electroexfoliationofgraphitetographeneinanaqueoussolutionofinorganicsaltandthestabilizationofitsspongestructurewithpolyfurfurylalcohol