Plasma-chemical synthesis of nanopowders based on copper oxide and metal-organic framework structures was carried out using low-pressure arc discharge plasma. The study of the obtained material was carried out by several methods (XRD, FTIR, TEM, TGA and EIS). TEM showed that the obtained powder is highly agglomerated particles with an average particle size of 13 nm, and the crystalline ordering of nanoparticles with a large (about 2 nm) lattice parameter is clearly visible. XRD showed the presence of four crystalline phases corresponding to [Cu3 (BTC)2], Cu, Cu2O and CuO. XRD results are in good agreement with FTIR studies. The DTA curve demonstrates a continuous exothermic process associated with a number of features of plasma-chemical synthesis and the morphology of the obtained nanoparticles. The study of the electrochemical properties of the materials obtained by the method of impedance spectroscopy revealed an anomalous accumulation of electrical charges around the electrodes due to electrochemical reactions for [Cu3 (BTC)2], which are associated with various reactions involving copper species in the organic framework.