an8b02126_si_001.pdf (5.06 MB)
Scalable Production of Graphene Oxide Using a 3D-Printed Packed-Bed Electrochemical Reactor with a Boron-Doped Diamond Electrode
journal contribution
posted on 2019-01-23, 21:16 authored by Sean E. Lowe, Ge Shi, Yubai Zhang, Jiadong Qin, Shujun Wang, Alexander Uijtendaal, Jiqing Sun, Lixue Jiang, Shuaiyu Jiang, Dongchen Qi, Mohammad Al-Mamun, Porun Liu, Yu Lin Zhong, Huijun ZhaoAlthough graphene
oxide (GO) has shown enduring popularity in the
research community, its synthesis remains cost prohibitive for many
of its demonstrated applications. While significant progress has been
made on developing an electrochemical route to GO, existing methods
have key limitations regarding their cost and scalability. To overcome
these challenges, we employ a combination of commercially available
fused-deposition-modeling-based 3D printing and highly robust
boron-doped diamond with a wide electrochemical potential window
to fabricate a scalable packed-bed electrochemical reactor for GO
production. The scalability of the reactor along the vertical and
lateral dimensions was systematically demonstrated to facilitate its
eventual industrial application. Our current reactor is cost-effective
and capable of producing electrochemically derived GO (EGO) on a multiple-gram
scale. By oxidizing flake graphite directly in an 11.6 M sulfuric
acid electrolyte, the production of EGO was streamlined to a one-step
electrochemical reaction, followed by a simple water-wash purification.
Almost all of the converted graphite oxide can be recovered, and the
final mass yield is typically 155% of the starting graphite material.
The as-produced EGO is dispersible in water and other polar organic
solvents (e.g., ethanol and dimethylformamide) and can be exfoliated
down to predominantly single-layered GO. Through a detailed study
of the product intermediates, the graphite was found to first form
a stage III or higher graphite intercalation compound, followed by
electrochemical oxidation proceeding from the top of the packed graphite
bed down. The EGO can be easily deoxygenated with low-temperature
thermal annealing (<200 °C) to produce thermally converted
EGO with significantly enhanced conductivity, and its promising application
as a conductive nanofiller in lithium-ion battery cathodes was
demonstrated. The simplicity, cost-effectiveness, and unique EGO properties
make our current method a viable contender for large-scale synthesis
of GO.
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stage IIIas-produced EGOgraphite oxideproduct intermediates11.6 Mscalable packed-bed electrochemical reactormultiple-gram scalewater-wash purificationgraphene oxidegraphite intercalation compoundGraphene Oxideacid electrolytefused-deposition-modeling-based 3 D printing3 D-Printed Packed-Bed Electrochemical Reactorgraphite bedelectrochemical oxidation proceedinglithium-ion battery cathodeselectrochemical reactionboron-doped diamondelectrochemical routegraphite materialresearch communityconductive nanofillerBoron-Doped Diamond ElectrodeScalable ProductionapplicationEGO propertiesoxidizing flake graphite
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