Gas-Phase Generation of Zinc Sulfide Particles Using a Single-Source Precursor
Abstract
Nanometer-sized (20 to 40 nm) ZnS particles were produced in a flow reactor by gas-phase reaction of the single-source precursor Zn(S2CNEt2)2(TMEDA) , where TMEDA = tetramethylethylenediamine. The precursor was prepared by reaction of the dimer, (Zn(S2CNEt2)2)2, with two equivalents of TMEDA. The product was isolated in quantitative yield and characterized by a variety of spectroscopic techniques and by single-crystal X-ray diffraction in the solid state. Transparent, colorless prisms of empirical formula C16H36N4S4Zn crystallized by cooling a warm (60 deg C), saturated toluene solution to room temperature, in the orthorhombic crystal system, space group P2(1)2(1)2(1) with unit cell dimensions a = 8.785(1) A, b = 11.611(2) A, c = 23.321(2) A, z = 4, with R = 4.64%, Rw = 5.32% for 3262 independent reflections where F > 3.0 sigma (F). The structure of Zn(S2CNEt2)2(TMEDA) was monomeric and distorted octahedral in the solid state. The precursor was evaporated into the gas phase and reacted in a hot-wall reactor at temperatures of 500, 600, and 700 deg C resulting in the formation of ZnS particles X-ray diffraction showed phase-pure ZnS particles with crystallite sizes of 15 - 25 nm at all temperature studied. Thermogravimetric analysis, elemental analysis, and transmission electron microscopy suggested that the particles also contained sulfur derived from the precursor.
Document Details
- Document Type
- Technical Report
- Publication Date
- May 06, 1994
- Accession Number
- ADA279700
Entities
People
- A. Datye
- A. Gurav
- D. Zeng
- Mark J. Hampden-smith
- Q. Powell
Organizations
- University of New Mexico