18.11.2016 Views

Thesis - Oztek_Muzaffer_T_200508_MA

You also want an ePaper? Increase the reach of your titles

YUMPU automatically turns print PDFs into web optimized ePapers that Google loves.

determined by the start and end of a hydrogen-helium peak pair. The flow rate through<br />

the reactor was monitored with a Fisher Scientific digital flowmeter.<br />

Dehydriding of the hydrided samples was accomplished by heating the reactor<br />

with heating tape up to 150 ºC under argon flow and analyzing the exit stream for<br />

hydrogen using the GC. As soon as no hydrogen was detected in the stream, the heating<br />

system was turned off to allow cool down to room temperature for the subsequent<br />

experiments.<br />

2.2.2.2. Activation procedure<br />

Samples ball milled in stainless steel vials with lower ball to powder ratios and longer<br />

milling times were activated in a high pressure reactor. Approximately 200 grams of<br />

milled alloy were placed in a Pyrex Petri dish that was then transferred into a 2000 mL<br />

capacity Parr Pressure Reactor. Pressure was monitored with one Omega type px303<br />

pressure transducer with a range up to 34 atm. Temperature in the reactor was regulated<br />

by a Love Controls Series 2600 type controller. Pressure and thermal data were acquired<br />

with a Dell GX240 PC using Lab View software through a National Instruments board.<br />

Samples were heated up to 250 ºC under a hydrogen pressure of approximately 20 atm.<br />

After the system reached equilibrium, the heating system was turned off and the system<br />

was allowed to cool under hydrogen pressure. After cooling, the system was vented and<br />

a heating cycle was run to remove absorbed hydrogen.<br />

31

Hooray! Your file is uploaded and ready to be published.

Saved successfully!

Ooh no, something went wrong!