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Thesis - Oztek_Muzaffer_T_200508_MA

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The dehydriding procedure was initiated immediately after the system reached<br />

ambient temperature at the end of hydriding process. For this procedure, the exit valves<br />

were opened to release hydrogen and a minimal argon flow was established using the<br />

needle valves. The system was purged with argon for 15 minutes after which the inlet<br />

valves were closed followed very quickly by closing the exit valves to maintain<br />

atmospheric pressure argon within the system. Dehydriding was accomplished by holding<br />

the furnace at the initial temperature for 180 seconds and then heating to T 2 with a ramp<br />

rate of 5 °C/min. The furnace was held at T 2 for 180 seconds and then cooled at a rate of<br />

10 °C/min. Dehydriding in a closed system allowed quantization of the H 2 given off by<br />

the sample. Hydriding and dehydriding cycles were repeated without removing the<br />

sample from the DSC.<br />

Because LaNi 5 and LaNi 5 Al x will absorb and release H 2 at ambient temperatures,<br />

their dehydriding characteristics were determined using a slightly modified procedure.<br />

For these samples, excess H 2 pressure after the hydriding experiment was reduced to 1<br />

atm. Then pressure and thermal data acquisition were started immediately. The system<br />

was heated to 150 ºC with no delay period.<br />

2.2.1.2. Thermal Activation Procedure<br />

Some samples were not sufficiently activated by ball milling alone. The activation<br />

of these samples was accomplished by a thermal cycle in the DSC following milling.<br />

This was done by placing the sample in the DSC in a hydrogen atmosphere at<br />

28

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