It has been tried to develop Ti-Ca alloys which demonstrates corrosion resistance in an aqueous fluoride solutions. The Ti-Ca alloys were produced by diffusion-metallizing method. A Ti plate and Ca grains were put in a sealed container of stainless steel. As the container was heated at 1000 oC, Ca was melted and partially vaporized in the inner space. Ca then contacts and permeats into the Ti plate to metallize. In a holding time of 450 h, the alloy surface consisted of two layers, the first was oxide layer and the second was metal layer of about 200 m thick. A Vickers micro hardness of the second layer was quite large, upto about 600 Hv. Evaluation of corrosion resistance for the second layer and the inner part was carried out by electrochemical potentiokinetic method. Test solutions were aqueous fluoride solutions produced with HF and NaF. A concentration of fluoride ion was fixed to 0.024 kmol m-3, and pH of the solution was varied from 3.4 to 4.7. As a result, both Ti and Ti-Ca alloy were passivated under natural immersion condition in the solution of pH 4.7. At pH 3.4, on the other hand, Ti was actively dissolved, but Ti-Ca alloy was still passivated, that means Ti-Ca alloy performs much better corrosion resistance than Ti.