To solve the problem of silicide coatings on tantalum substrates failing due to elemental diffusion under high-temperature oxidation environments and to find diffusion barrier materials with excellent effects of impeding Si elemental spreading, TaB₂ and TaC coatings were prepared on tantalum substrates by the encapsulation and infiltration methods, respectively. Through orthogonal experimental analysis of the raw material powder ratio and pack cementation temperature, the best experimental parameters for the preparation of TaB₂ coatings were selected: powder ratio (NaF:B:Al₂O₃ = 2.5:1:96.5 (wt.%)) and pack cementation temperature (1050 °C). After diffusion treatment at 1200 °C for 2 h, the thickness change rate of the Si diffusion layer prepared using this process was 30.48%, which is lower than that of non-diffusion coating (36.39%). In addition, the physical and tissue morphological changes of TaC and TaB₂ coatings after siliconizing treatment and thermal diffusion treatment were compared. The results prove that TaB₂ is a more suitable candidate material for the diffusion barrier layer of silicide coatings on tantalum substrates.