Sustainable Synthesis of High-Surface-Area Graphite Oxide via Dry Ball Milling

Abstract

A sustainable route to produce graphite oxide (GO) is presented using dry ball milling. The production method was based on pristine graphite flakes in a planetary ball mill. The prepared GO was characterized using UV–vis spectroscopy, BET surface area analysis, thermal analysis, SEM-EDX, TEM, XPS, elemental analysis, and Raman spectroscopy. The degree of graphite oxidation was controllable by the milling time and milling material, and the carbon-based yields ranged from 86 to 97%. The maximum oxygen/carbon ratios of the produced GOs were 0.16 and 0.15 after 24 h of ball milling with steel and zirconia balls, respectively. The BET surface area increased with increasing milling time from 1 m2 g–1 for pristine graphite up to 730 m2 g–1 for the ball-milled samples. Furthermore, the intensity ratios of the D and G bands (I D /I G ) from the Raman spectra were 0.84 and 0.77 for GO produced with the steel and zirconia balls, respectively. The in-plane sp2 crystallite sizes (L a) of graphite (168 nm) decreased to 20 (steel balls) and 22 nm (zirconia balls). Additionally, the produced GO was tested as an adsorbent for methylene blue dye removal.

Mechanochemical Routes to Functionalized Graphene Nanofillers Tuned for Lightweight Carbon/Hydrocarbon Composites

“…This is in accordance with observations reported by Mahmoud et al. who ball‐milled graphite under an air atmosphere . Moreover, the high nitrogen content of 2.1 wt% (+420% with respect to MFG‐Ar) indicates that also nitrogen reacted with the carbon upon milling under air.…”

“…According to Mahmoud et al. dry ball‐milling of graphite the presence of air using steel and zirconia balls holds prospects regarding the sustainable synthesis of high‐surface graphite oxide useful as polymer additive and as an adsorbent for methylene blue dye removal . Typically, Jeon et al.…”

“…[96] As a sustainable alternative route to graphene oxide formation via the graphite oxide intermediate, ball-milling of graphite in the presence of oxygen was reported to yield hydroxyl-functionalized graphene stacks which did not form single-and few-layer graphene oxide dispersions upon shearing but met the demand for applications like adsorbents. [100] The addition of magnesium during ball-milling of graphite oxide was employed to mechanochemically reduce graphene oxide. [101] Alternatively, hydrogen addition is used in mechanochemical reduction of graphene oxide.…”

“…[101] Alternatively, hydrogen addition is used in mechanochemical reduction of graphene oxide. [102] Meanwhile an extraordinarily wide range of MFG bearing hydroxyl, carboxylic acid, halogen, five-,and six-membered N-heterocycles, sulfonic acid, and even phosphate groups have been prepared via graphite mechanochemistry in the presence of gases like CO 2 , [96,99] N 2 , [103,104] NH 3 , [105] H 2 , [106] O 2 , [100] Cl 2 , [107] F 2 , [107] and SO 2 , [99] liquids like Br 2 , [106,107] H 2 O, [108] SO 3 , [99,109] CO 2 /SO 3 , [99] as well as solids like red phosphorous, [110,111] sulfur, [112][113][114][115] melamine, [116][117][118][119] urea, [104,120,121] KOH, [122] NaCl, [123] Mg, [101] Fe, [124] Si, [125][126][127] polystyrene, [128] cellulose, [64] chitin, [129] polyvinylpyrrolidone, [130] polyetherketone, [131] and I 2 . [106,…”

Covalent Bonding of PANI and p‐Phenylenediamine‐Functionalized GO Using N,N′‐Dicyclohexylcarbodiimide as Dehydrating Agent for Electrochromic Applications

“…Raman spectra of graphite, GO, PANI and PANI‐GO nanocomposite are illustrated in Figure . Two important characteristic peaks of graphite, D and G bands appear at 1347 cm −1 and 1597 cm −1 , respectively . The D band is caused by the defects, edge areas or disordered carbon, whereas the G band that arises in the zone center E 2g mode is related to the vibration of sp 2 ‐hybridized carbon.…”