We have developed a simple, efficient, cost-effective, and reproducible method on simultaneous dispersion of CuO nanoflowers and semi-spherical nanoparticles onto multi-walled carbon nanotube (MWCNT) surface. It makes use of a combination of Infrared (IR) irradiation, in situ-generated diazonium salt, mechanical mixing, and calcination. To achieve this nanocomposite, 5-amino-1,2,3-benzenetricarboxylic acid is chosen as a dispersing agent and cupric acetate as a CuO precursor. The process also involves calcination at moderate temperature (200 degrees C). The resulted nanohybrid was characterized utilizing PXRD, XPS, TEM, FESEM, and EDS techniques. The obtained nanoparticles exhibit two different shapes and sizes: as flowers with approximate to 33-170-nm size range and semi-spherical form with sizes in the approximate to 4-15-nm range. They are homogeneously distributed and firmly anchored on the MWCNT surface. The method can be applied to prepare material on a large scale. They are expected to have applications in electrochemical sensors, catalysis, energy systems, etc.