LITHIUM NITRIDE → Zirconium chloride (ZrCl4), (T-4)-

A mortar and pestle was used to mix 4.434 gram of zirconium tetrachloride (ZrCl4) and 0.882 gram of lithium nitride (Li3N) in order to form the reactant mixture with a stoichiometric ratio of Li3N to ZrCl4 of 4/3. The reactant mixture was placed in a 45 milliliter stainless steel container. A screw top cap was placed on the stainless steel container. The screw top cap had two insulated leads protruding therethrough, which held a nichrome filament in the reactant mixture. An external electric charge was applied to the leads for no more than two seconds thereby igniting the reactant mixture. The resulting yellow-brown product was washed with methanol, dried and then ground with a mortar and pestle. The product was further washed with ten percent nitric acid, methanol, water and acetone on a vacuum filter. The powder was then dried on a vacuum line. The resulting light-brown product was pure ZrN with a cubic lattice spacing of 4.57 Angstroms as determined by X-ray powder diffraction. Use of the Scherrer equation gave a calculated particle size of 500-600 Angstroms. The product yield was ninety-one percent (1.822 grams out of 1.998 grams theoretically possible). A pressed disc indicated metallic type conductivity. A balanced equation is as follows:

ORD record

ord-d11e6cd4833e41488413300aeb366076

Source dataset

uspto-grants-1992_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05110768