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DESIGN, ASSEMBLY AND CHARACTERIZATION OF COMPOSITE ...

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theoretical density with well-controlled microstructure. Rheological measurements are<br />

used to determine optimal dispersant concentration for ink preparation. After creating a<br />

stable Ni suspension at a solid volume fraction φsolids = 0.57, the suspension is flocculated<br />

to achieve a colloidal gel at φsolids = 0.472. Again, rheological measurements are used to<br />

assess flow behavior after flocculation. Thermogravimetric analysis (TGA) is used to<br />

estimate residual carbon content in sintered Ni. Hardness measurement and<br />

metallography of sintered nickel structures are presented as measures of the final product<br />

properties. Finally, fabricated objects of various shapes using nickel ink are demonstrated.<br />

4.2. Experimental Section<br />

4.2.1. Materials<br />

A near-spherical shaped nickel powder (ENP 800, Umicore, Fort Saskatchewan,<br />

Alberta, Canada), with a mean particle size 0.8 µm and theoretical density of 8.908 g/cm 3 ,<br />

is used as the colloidal phase. The manufacturer assay reports a tap density of 4.0 g/cm 3 ,<br />

0.15% carbon (proprietary polymer used by manufacturer for powder synthesis) and 0.6%<br />

oxygen by weight, and specific surface area 0.9 m 2 /g. A 50% by weight aqueous solution<br />

of polyethylenimine (PEI) with MW 2k (PEI-2K) (Cat # 408700, SigmaAldrich,<br />

Milwaukee, WI), a branched PEI with MW 25k (PEI-25K) (Cat # 408727, SigmaAldrich,<br />

Milwaukee, WI), and a 50% by weight aqueous solution of branched PEI with MW 50k-<br />

100k (PEI-50K) (ICN Biomedical, Aurora, OH) are compared for use as dispersant. An<br />

40% by weight aqueous solution of the ammonium salt of poly(acrylic acid) (PAA)<br />

(Darvan 821A, R.T. Vanderbilt Co., Norwalk, CT) is used as the flocculant.<br />

Hydroxypropyl methylcellulose (HPMC) (Methocel F4M, Dow Chemical Company,<br />

114

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