Static sublimation purification process and characterization of LiZnAs semiconductor material

• Published in: Journal of crystal growth 2016-03, Vol.438 (C), p.99-103
• Main Authors: Montag, Benjamin W., Reichenberger, Michael A., Edwards, Nathaniel S., Ugorowski, Philip B., Sunder, Madhana, Weeks, Joseph, McGregor, Douglas S.
• Format: Article
• Language: English
• Subjects: A1. Purification; A1. Radiation; A1. X-ray diffraction; B1. Lithium compounds; B2. Semiconducting ternary compounds; Devices; Impurities; Lithium; Neutron detectors; Quartz; Semiconductor materials; Semiconductors; Sublimation
• ISSN: 0022-0248; 1873-5002
• DOI: 10.1016/j.jcrysgro.2015.12.023

Refinement of the class AIBIICV materials continue as a candidate for solid-state neutron detectors. Such a device would have greater efficiency, in a compact form, than present day gas-filled 3He and 10BF3 detectors. The 6Li(n,t)4He reaction yields a total Q value of 4.78MeV, larger than 10B, and easily identified above background radiations. Hence, devices composed of either natural Li (nominally 7.5% 6Li) or enriched 6Li (usually 95% 6Li) may provide a semiconductor material for compact high efficiency neutron detectors. A sub-branch of the III–V semiconductors, the filled tetrahedral compounds, AIBIICV, known as Nowotny–Juza compounds, are known for their desirable cubic crystal structure. Starting material was synthesized by equimolar portions of Li, Zn, and As sealed under vacuum (10−6Torr) in quartz ampoules with a boron nitride lining, and reacted in a compounding furnace [1]. The synthesized material showed signs of high impurity levels from material and electrical property characterization. In the present work, a static vacuum sublimation of synthesized LiZnAs loaded in a quartz vessel was performed to help purify the synthesized material. The chemical composition of the sublimed material and remains material was confirmed by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). Lithium was not detected in the sublimed material, however, near stoichiometric amounts of each constituent element were found in the remains material for LiZnAs. X-ray diffraction phase identification scans of the remains material and sublimed material were compared, and further indicated the impurity materials were removed from the synthesized materials. The remaining powder post the sublimation process showed characteristics of a higher purity ternary compound. •LiZnAs in-house synthesized material was purified by a static sublimation process.•The product kept the desired ternary stoichiometric ratio (1:1:1).•A powder XRD pattern of the sublimed material matched with zinc arsenide (Zn3As2).•The purified XRD pattern corresponded to what was found in the literature.•A lattice constant of 5.901±0.002Å was determined for purified LiZnAs.