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Thesis - Oztek_Muzaffer_T_200508_MA

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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

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