Journal
CHEMISTRY OF MATERIALS
Volume 24, Issue 7, Pages 1276-1282Publisher
AMER CHEMICAL SOC
DOI: 10.1021/cm203223z
Keywords
graphene; graphite oxide; graphene oxide; intercalation compound; mechanism; decomposition
Funding
- Cluster of Excellence Engineering of Advanced Materials at the University of Erlangen-Nuremberg
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The formation, stability, and decomposition of CO, intercalated graphene oxide was analyzed by FTIR, TGA-MS, TGA-IR, AFM, and SEM for the first time. We found that the formation starts at 50 degrees C and develops up to 120 degrees C. The formation process can be best observed by FTIR spectroscopy, and the product is stable at ambient conditions. At higher temperatures, the decomposition of CO2 intercalated graphene oxide occurs due to the release of water, CO2, and CO that can be monitored by TGA-MS and TGA-IR analysis. AFM and SEM images can visualize the formation of blisters in GO films that become instable at 210 degrees C. We further prepared graphene oxide with a low water-content and found that the formation of CO2 was significantly suppressed and CO became the major species responsible for the weight loss. In addition we prepared (OH2)-O-18 treated graphene oxide to elucidate the formation process of CO2 and found (COO)-O-16-O-18 by TGA-MS analysis that proves the crucial role of water daring CO2 formation. From these experiments we propose that hydrate species are key-intermediates for the formation of CO2, Hence, it seems likely that rearrangement reactions that can proceed via hydrate intermediates, known from organic chemistry, are probably responsible for the formation of carboxylic acids at the edges of graphene oxide sheets after sonication of graphite oxide. Further, our investigations prove that graphene oxide is less stable than shown by TGA measurements. This has a high impact on the electronic properties of reduced graphene oxide, especially for all those using it for electronic applications.
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