Method for treating titanium objects with a surface layer of mixed tantalum and titanium oxides
View Patent ↗This invention introduces a method for treating a surface of an electrically conductive object with a refractory metal. In one embodiment, the refractory metal is tantalum and the object is a titanium substrate. A surface layer of mixed tantalum and titanium oxides is created by first heating the object and tantalum chloride in a reaction chamber and subsequently heat treating the object in an oxygen containing environment. The electrically conductive object can in a non-limiting way be DSA solutions (Dimensionally Stable Anodes), fuel cells or connector plates.
1. A method for alloying a titanium surface of an electrically conductive object with a refractory metal to obtain an alloyed surface of titanium and refractory metal, said alloyed surface having an increasing gradient towards titanium into the internal of the object, said process comprising the steps:
placing the object and a refractory metal halide in a reaction chamber of a furnace,
heating the object in the reaction chamber at a target temperature over a first time period,
cooling the reaction chamber over a second time period, and
removing the object from the reaction chamber,
wherein the refractory metal halide is TaCl5 and the tantalum is precipitated using the net reaction 4 TaCl5(s)+5 Ti(s)→4 Ta(0)+5 TiCl4(g), where Ta(0) indicates that tantalum is present in oxidation state zero.
2. The method as in claim 1 , wherein the supplied tantalum pentachloride is solid tantalum pentachloride.
3. The method as in claim 2 , wherein the first time period is 3-5 minutes.
4. The method as in claim 3 , wherein the tantalum pentachloride is supplied to the reaction chamber in the form of a powder or an ampoule exploding in the reaction chamber.
5. The method as in claim 1 , wherein the formed TiCl4 is removed by pumping, freezing, condensing or through a passive outlet.
6. The method as in claim 1 , wherein the temperature for the first time period is within 880-1200 degrees Celsius.
7. The process as in claim 6 , wherein the temperature for the first time period is between 915-930 degrees Celsius.
8. The method as in claim 1 , where the object subsequent to the second time period is heated in an oxidizing atmosphere after it has been removed from the reaction chamber.
9. The method as in claim 1 , where oxidizing compounds are added to the reaction chamber before or during the first time period.