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This work reports an innovative approach to the fabrication of free-standing thin films of multiwalled carbon nanotubes (MWCNTs)/graphene oxide (GO) nanohybrids by using dimethyl formamide (DMF) and n-hexane as a solvent–antisolvent system for the growth of thin films of MWCNTs/GO nanohybrids. The synthesis of the GO was carried out by using the modified Hummers method, while the synthesis of MWCNTs/GO nanohybrids was done by the intermixing of the carboxylic acid functionalized MWCNT and GO using the solution-mixing method. The growth of the thin film of MWCNTs/GO nanohybrids was done by obeying the surface-tension-driven phenomena which occur mainly due to the coalescence of bubbles due to the solvent–antisolvent interfacial tension. Furthermore, density functional theory (DFT)-based first-principles simulations were performed to understand the structural, electronic, and capacitive aspects of MWCNT/GO nanohybrids. The computational results demonstrated excellent quantum capacitance in the MWCNT/GO nanohybrid electrodes. Inspired by the computational results, the same process elaborated above has also been employed to develop binder-free supercapacitor devices utilizing the MWCNT/GO nanohybrid as an electrode material. The electrochemical performance of this electrode in 1 M aqueous H2SO4 demonstrates a good energy density of 21.63 WhKg−1 at a current density of 0.5 Ag−1, with a high specific capacitance of 369.01 F/g at the scan rate of 2 mVs−1 and excellent cyclic stability of 97% for 5000 charge–discharge cycles.