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This paper aims to improve the aqueous stability and electrochemical activity of HKUST-1 (or Cu3(BTC)2, BTC = benzene 1,3,5-tricarboxylate; and HKUST from Hong Kong University of Science and Technology) by the incorporation of Graphene Oxide (GO). The synthesis was carried out in two steps; first, CuII ions were pre-adsorbed on the surface of GO, and then the BTC organic linker was added to form the HKUST-1 structure dispersed on GO sheets. Two concentrations of copper were used in the synthesis, 3.57 and 14.27 mmol, to obtain the samples: GO@HKUST-1low and GO@HKUST-1high, respectively. N2 adsorption properties of GO@HKUST-1high suggest an increase in surface area compared to HKUST-1 up to 1082.0 m2·g−1. In addition, the CO2 capture of GO@HKUST-1high increased from 5.34 (HKUST-1) to 6.92 mmol·g−1 at 273 K and 100 kPa. This improvement is associated with the dispersion of the HKUST-1 on the GO sheets achieved through the synthesis strategy used, which also increased the surface area, H2O adsorption capacity of the composite material, and electrochemical stability. After the H2O adsorption tests, XRD confirmed that the material was stable under aqueous conditions, showing that the material did not undergo any structural modification. [ABSTRACT FROM AUTHOR]