Mesoporous 2D nanoflakes architectures of mono- and bi-metallic cobalt and nickel hydroxide (meso-Co-Ni(OH)2) hybrids were synthesized using novel chemical precipitation of foam-surfactant liquid crystal dual template (FSDT). The dissolved cobalt and nickel ions within the aqueous region of the Brij®78 surfactant template was reduced by the excess of sodium borohydride reducing agent that simultaneously generates excessive hydrogen foam as a double template. The physicochemical characterizations of the mono- and bi-metallic nanostructured Co-Ni(OH)2 hybrids performed using X-ray diffraction, surface area analyzer, scanning and transmission electrons microscopic techniques showed the formation of highly mesoporous hydroxides 2D nanoflakes architectures having an amorphous structure and surface area up to 253.50 m2/g. The electrochemical and supercapacitance evaluation of the mono-, and bi-metallic mesoporous hydroxides showed excellent Faradaic supercapacitance performance within a wider potential window and a higher charge and discharge rate. In particular the mesoporous monometallic of Co(OH)2, Ni(OH)2, bimetallic Co-Ni(OH)2 with Co/Ni ratios of (1:1), and (1:3), hydroxides showed total capacitances of 204, 869, 943, and 1384, F/g at charging current density of 5.0 A/g respectively and capacity retention rate of approximately 99.4% after 300 cycles. This suggests that these materials hold promise as electrode materials for energy storage applications.