Posted on by maxfomitchev

The most straightforward way to make titanium deuteride powder is to heat titanium sponge to ~350-450°C in D2 atmosphere. Once this temperature is reached titanium will react with deuterium gas rapidly through an exothermic reaction Ti + D2 = TiD2.

In order to accomplish this reaction I have built an experimental setup with the block diagram shown on Fig. 1. The actual setup is shown on Fig. 2.

Fig. 1.Titanium deuteride synthesis process block diagram.
Fig. 2. Titanium deuteride synthesis reactor.

I have deposited 1 lb of 325-mesh titanium sponge into an aluminum gas cylinder mounted to a simple vacuum manifold comprising a leak valve for initial evacuation, a Pfeiffer APR 265 pressure gauge (connected to Pfeiffer TPG262 gauge controller), and a gas inlet connected to a 50L dueterium lecture bottle via a regulator. I have mounted a 375W / 120V AC heat strip driven by a variac (to regulate power) at the bottom of the cylinder. I have also used an external thermocouple wedged between the heat strip and the cylinder to monitor the temperature.

My gas loading protocol was as follows:

  1. After depositing titanium sponge into the cylinder, I have evacuated the cylinder by connecting the leak valve to a vacuum pump to remove air;
  2. I admitted the initial charge of about 1000 Torr of D2 into the cylinder and set the lecture bottle regulator to maintain this pressure;
  3. I turned on the heat strip and allowed temperature to rise slowly to 450°C. As the temperature was rising so was the pressure inside the cylinder: it reached about 1500 Torr;
  4. When my externally mounted thermocouple was reading 450°C for a few minutes the titanium sponge inside the cylinder warmed up sufficiently to start the Ti+D2 reaction; I could tell that the reaction started by seeing pressure drop slightly, at which point the regulator engaged and I could tell that deuterium gas was flowing by hearing the regulator clicking and observing slight pressure fluctuation reported by the vacuum gauge controller;
  5. It is amazing how much deuterium 1 lb of titanium sponge consumes: I have gone through 100L of D2 to fully saturate the sponge; when the sponge is fully saturated deuterium is no longer consumed, the regulator quits clicking and the pressure remains stable. At this point I turned off the heat and allowed the system to cool.

The resulting TiD2 powder is shown on Fig. 3. It is a rather fine black dust, characteristic of titanium hydride.

Fig. 3. TiD2 powder.

You can buy your TiD2 powder here.