Utilising the hydrodynamics of thin film flow over a spinning disc for graphene exfoliation
File(s)
Author(s)
Uzo, Nwachukwu
Type
Thesis
Abstract
Graphene, a 2D nanomaterial, has remarkable mechanical, electrical, thermal and optical properties, which has the potential to transform the technological landscape. Methods currently
available for graphene production are not at an industrial scale, with rates rarely exceeding
0.04 g/h. This thesis investigates the use of the spinning disc as a vehicle for the scale-up of
graphene production by linking how the hydrodynamics of the spinning disc impacts liquid phase exfoliation.
High speed imaging results identifi ed the
flow regime showing that it is as a direct result from the balance of the key forces (inertia, surface tension and viscosity). The regimes identi ed were smooth, spiral, transition to 3D and fully 3D waves. Increasing the body force relative
over surface tension and viscosity stipulates a change in regime suggesting a critical Reynolds
number is needed to be exceeded locally on the disc for each of the flow regime.
Both 2D and 3D direct numerical simulations further reinforced this interplay between the
forces and established that the spiral wave regime could not generate enough local shear rate to exceed the critical needed for exfoliation of 104 s-1 which will be predominantly governed
by the 3D regime.
Graphene exfoliation was governed by the hydrodynamics in particular related to the shear
rate and residence time which determined the yield of about 0.25 wt % with natural graphite
precursor for the highest shear rate after 6 hours of processing. Shear rate was also found to
impact lateral size and selectivity with the highest shear giving sizes between 0.1 - 5 micro m and
selectivity of 90 % to 1 - 4 layers. The Raman ID/IG ratio of 0.14 and ID/ID' of 1.8 suggested
it was mostly edge defects that were present implying high quality graphene was produced. To
further reduce the interlayer cohesive energy to expedite the exfoliation process, pre-processing
the graphite either via pre-sonication or ball-milling was carried which led to an increase of
the yield to 1.1 wt % (production rate of 0.01 g=h) however some of the graphene sheets were
wrinkled due to the introduction of the ball milling.
available for graphene production are not at an industrial scale, with rates rarely exceeding
0.04 g/h. This thesis investigates the use of the spinning disc as a vehicle for the scale-up of
graphene production by linking how the hydrodynamics of the spinning disc impacts liquid phase exfoliation.
High speed imaging results identifi ed the
flow regime showing that it is as a direct result from the balance of the key forces (inertia, surface tension and viscosity). The regimes identi ed were smooth, spiral, transition to 3D and fully 3D waves. Increasing the body force relative
over surface tension and viscosity stipulates a change in regime suggesting a critical Reynolds
number is needed to be exceeded locally on the disc for each of the flow regime.
Both 2D and 3D direct numerical simulations further reinforced this interplay between the
forces and established that the spiral wave regime could not generate enough local shear rate to exceed the critical needed for exfoliation of 104 s-1 which will be predominantly governed
by the 3D regime.
Graphene exfoliation was governed by the hydrodynamics in particular related to the shear
rate and residence time which determined the yield of about 0.25 wt % with natural graphite
precursor for the highest shear rate after 6 hours of processing. Shear rate was also found to
impact lateral size and selectivity with the highest shear giving sizes between 0.1 - 5 micro m and
selectivity of 90 % to 1 - 4 layers. The Raman ID/IG ratio of 0.14 and ID/ID' of 1.8 suggested
it was mostly edge defects that were present implying high quality graphene was produced. To
further reduce the interlayer cohesive energy to expedite the exfoliation process, pre-processing
the graphite either via pre-sonication or ball-milling was carried which led to an increase of
the yield to 1.1 wt % (production rate of 0.01 g=h) however some of the graphene sheets were
wrinkled due to the introduction of the ball milling.
Version
Open Access
Date Issued
2019-09
Date Awarded
2020-03
Copyright Statement
Creative Commons Attribution NonCommercial Licence
Advisor
Matar, Omar
Petit, Camille
Sponsor
European Commission
Imperial College London
Grant Number
707340
Publisher Department
Chemical Engineering
Publisher Institution
Imperial College London
Qualification Level
Doctoral
Qualification Name
Doctor of Philosophy (PhD)