The authors conducted a comparative study on the kinetics of electrochemical plating (Fig. 1, 3) and properties of gold coating performed upon gallium arsenide samples with cyanide and sulphite-thiosulphate electrolytes at 20-67℃ (Table 1). According to polarization studies, the chemical composition of gold compounds, reduced upon cathodes at various potentials, differs (Fig. 2). Potentials above -0.4 V stipulate the fact that gold reduction from sulphite-thiosulphate solutions occurs under activation control. Potentials ranging from -0.4 to -0.7 V cause the activation energy of gold reduction equals 20 kJ/mol, which indicates the diffusion-based kinetics of the process (Fig. 4). It was established that under the current density 3.5 mA/cm2, the overpotential deposition of gold from sulphite-thiosulphate electrolyte is lower, compared to that of gold from cyanide solutions; under the current density 4 mA/cm2, the overpotential deposition of gold from sulphite-thiosulphate electrolyte is higher, compared to that of gold from cyanide solutions (Fig. 3). Gold layers deposited upon gallium arsenide samples from sulphite-thiosulphate electrolyte are characterized by lower parameters of surface roughness, compared to gold layers deposited from cyanide electrolyte. In the case of layer thickness 6 mkm, Ra of coatings deposited from sulphite-thiosulphate was equal to 60 nm; Ra of coatings deposited from cyanide electrolyte, 90 nm (Fig. 5). Gold deposition from sulphite-thiosulphate electrolyte, in contrast to deposition from acidic cyanide electrolyte, does not induce degradation of positive photoresist materials, thus it can be used for producing gold coatings with vertical walls (Fig. 6).