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

A mortar and pestle was used to mix 0.991 gram of zirconium tetrachloride (ZrCl4) and 0.204 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 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, water and acetone on a vacuum filter. The powder was then dried on a vacuum line. The resulting 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 200-250 Angstroms. See Elements of X-ray Diffraction written by B. D. Cullity, Addison-Wesley, Reading, Mass., 1956. The product yield was fifty five percent (0.2488 gram out of 0.4475 gram theoretically possible). A pressed disc indicated metallic type conductivity. A balanced equation is as follows:

ORD record

ord-501713b49888463daafd854400fe500f

Source dataset

uspto-grants-1992_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05110768