Metal-organic frameworks (MOFs) as an emerging kind of poriferous crystalline compounded material, the preparation and applications including gas storage, [1,2] catalysis, [3] separation, [4] drug delivery, [5,6] and chemical sensors [7] of its new porous structure has achieved tremendous development in the past few decades. Co8-MOF-5 was first reported as electrode materials for supercapacitors (SCs). MOFs with large specific surface area attribute to high rate of holes that can reserve ample electric charge and promote the dispersion of electrolyte ions as well as provide plentiful faradaic redox centers. [8] Therefore, more and more MOFs used as electrode materials have been rapidly developed. It was Yang et al. first published that a 2D nickel-based MOF has excellent current capability (providing a high specific volume of 1127 F g À1 at 0.5 A g À1 ) and outstanding cycle durability (over 90% capacitance retention after cycling 3000 times). [9] The synthesis of unique flower-like structure Ni-MOFs has been reported, which produced a high pseudo capacity of 1457.7 F g À1 at 1 A g À1 . [10] However, currently, most Ni-MOFs with high capability and unique morphology are synthesized by solvothermal method. On various occasions, solvothermal requires a long reaction time of up to several days. Moreover, the reaction of the frame members must be carried out at high temperatures (usually 373-523 K) and pressure (1-10 MPa). Considering the great capability of MOFs to be used in SCs in the future, some more effective and new synthesis techniques for substitution should be developed as soon as possible. What is more, the adoption of high-duty ultrasound (US) can provide a convenient, environmental, and commonly used compositing tool for MOFs materials.US causes chemical changes based on cavitation phenomena, involving the sequential generation, rising, and succedent collapse of bubbles in hot spots. [11][12][13] More specifically, when radiated by the US, the alternating expansion sound wave and compression sound wave will produce bubbles, and the vibratory blisters can amass US power to a particular amount (tens of millimeters). The bubbles will grow excessively in a very short life (heating and cooling rates > 1010 K s À1 ) and then collapse. [14][15][16] A great concentration of energy was obtained in the course of the eruption, bringing a certain temperature at a certain part of about 5000 K and a pressure of about 1000 bar. This power will be diffused into the surroundings during the collapsing, so the temperature of the gas at the important point will quickly renew to the value of the surroundings and its rates of heating/cooling will return to up 1010 K s À1 . [17] Because of such factors, US irradiation make it possible to get sufficient amounts of energy to achieve the reaction which is previously hard to get with other approaches. even macroscopically at room temperature. In detail, the first synthesis material came into being in 2008 by Qiu et al. with (Zn 3 BTC 2 12H 2 O). [18]