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DESIGN, ASSEMBLY AND CHARACTERIZATION OF COMPOSITE ...

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At the beginning of each firing procedure, two cycles of vacuuming and flushing<br />

are used to purge air out of the tube furnace. A mass flow controller (Tylan FC-260,<br />

Entegris, Chaska, Minnesota) with a maximum flow rate of 200 standard cubic<br />

centimeters per minute (sccm) at room temperature is used for controlling the processing<br />

gas flow rate. A 5% H2, 95% N2 mixture is bubbled through water contained in a flask<br />

and then fed through the tube furnace. By adjusting flow rate, oxygen partial pressure in<br />

the tube furnace may be adjusted to prevent Ni oxidation with negligible reduction of BT.<br />

A typical flow rate is in the range from 50-100 sccm. An oxygen probe (DS, Australian<br />

Oxytrol Systems, Eaglehawk, Victoria, Australia) is used to monitor oxygen partial<br />

pressure above the sample. After that, the post firing diameter is measured at mid-length<br />

point of each rod using a micrometer.<br />

Figure 5.1 Temperature profiles for firing rod-shaped specimens, with the same heating<br />

ramp rate for all specimens at 5 °C/min, and no isothermal hold.<br />

142

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