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DESIGN, ASSEMBLY AND CHARACTERIZATION OF COMPOSITE ...

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thickness. Each layer of the structure consists of a parallel array of filaments printed in a<br />

serpentine pattern and aligned with the x or y axis in alternating layers. For comparison<br />

purpose, also used are Ni(m) inks that have the same BT:Ni ratios and solid volume<br />

fraction but no LiAC∙2H 2O addition. These BT-Ni inks are similar to those described in<br />

Chapter 5, so the details of composition and processing are not repeated here.<br />

After drying, binder burnout is performed at 260 °C in a tube furnace<br />

(Thermolyne F21100, Barnstead International, Dubuque, Iowa) for 8 hours. Subsequently,<br />

specimens of each composition are fired in a tube furnace (GSL 1600X, MTI Corporation,<br />

Richmond, CA) to peak temperature at 700 °C, 800 °C, 900 °C, and 1000 °C with an<br />

isothermal hold of 2 hour, and then cooled down to room temperature. Heating ramp rate<br />

is 5 °C/min. At the beginning of each firing procedure, two cycles of vacuuming and<br />

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

260, 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. The 5H2/95N2 mixture is bubbled through water and then fed through the<br />

tube furnace. By adjusting its flow rate, oxygen partial pressure in the tube furnace may<br />

be adjusted to prevent Ni from oxidation with negligible reduction to BT. A typical flow<br />

rate is in the range from 50-100 sccm.<br />

6.2.5. Fabrication of BT-Ni Composites<br />

Specimens with abrupt transitions in composition are created by serial printing<br />

using the LFBT alongside Ni'(m) inks. Binder removal for the composites is carried out<br />

in air (Thermolyne F21100, Barnstead International, Dubuque, Iowa) for 8 hours at<br />

173

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