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. 2015 Jul 2:5:11807.
doi: 10.1038/srep11807.

In-Situ ESEM and EELS Observation of Water Uptake and Ice Formation in Multilayer Graphene Oxide

Takeshi Daio  1 , Thomas Bayer  2 , Tatsuya Ikuta  3 , Takashi Nishiyama  3 , Koji Takahashi  4 , Yasuyuki Takata  5 , Kazunari Sasaki  6 , Stephen Matthew Lyth  7
Affiliations

In-Situ ESEM and EELS Observation of Water Uptake and Ice Formation in Multilayer Graphene Oxide

Takeshi Daio et al. Sci Rep. .

Abstract

Graphene oxide (GO) is hydrophilic and swells significantly when in contact with water. Here, we investigate the change in thickness of multilayer graphene oxide membranes due to intercalation of water, via humidity-controlled observation in an environmental scanning electron microscope (ESEM). The thickness increases reproducibly with increasing relative humidity. Electron energy loss spectroscopy (EELS) reveals the existence of water ice under cryogenic conditions, even in high vacuum environment. Additionally, we demonstrate that freezing then thawing water trapped in the multilayer graphene oxide membrane leads to the opening up of micron-scale inter-lamellar voids due to the expansion of ice crystals.

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Figures

Figure 1
Figure 1
(a) Schematic image of the bespoke cold stage. The multilayer GO membrane is attached and the cross-section is exposed to the electron beam. (b) Photograph of the stage. (c) An SEM image of the multilayer GO membrane. (d) TEM images of a few-layer region of the multilayer GO membrane. The inset in (d) shows the structure at atomic resolution.
Figure 2
Figure 2
ESEM images of the cross-section of the multilayer GO membrane at (a) 30, (b) 40, (c) 50, (d) 60, (e) 70, and (f) 90 % RH. Schematic images of few-layer GO under (g) dry and (h) humidified conditions.
Figure 3
Figure 3
(a) Relative humidity and resulting thickness variation of the multilayer GO membrane with time. (b) Thickness versus relative humidity. (c) Average thickness at a given relative humidity, with second order fitting.
Figure 4
Figure 4
(a) SEM image of the multilayer GO membrane after freezing then thawing. (b) EELS spectra of GO at 40 °C and −160 °C. The peak at 8.5 eV, signifies the presence of crystalline ice. The peak at 5 eV is characteristic of GO.
See this image and copyright information in PMC

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