Accession Number:
ADA279700
Title:
Gas-Phase Generation of Zinc Sulfide Particles Using a Single-Source Precursor
Descriptive Note:
Technical rept.
Corporate Author:
NEW MEXICO UNIV ALBUQUERQUE DEPT OF CHEMISTRY
Personal Author(s):
Report Date:
1994-05-06
Pagination or Media Count:
32.0
Abstract:
Nanometer-sized 20 to 40 nm ZnS particles were produced in a flow reactor by gas-phase reaction of the single-source precursor ZnS2CNEt22TMEDA , where TMEDA tetramethylethylenediamine. The precursor was prepared by reaction of the dimer, ZnS2CNEt222, 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 P212121 with unit cell dimensions a 8.7851 A, b 11.6112 A, c 23.3212 A, z 4, with R 4.64, Rw 5.32 for 3262 independent reflections where F 3.0 sigma F. The structure of ZnS2CNEt22TMEDA 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.
Descriptors:
- *PRECURSORS
- *GAS ANALYSIS
- *PHASE
- *FLOW
- *ZINC
- *PARTICLES
- *SULFIDES
- *REACTOR OPERATION
- TEMPERATURE
- METHYL RADICALS
- SINGLE CRYSTALS
- ROOM TEMPERATURE
- ELECTRON MICROSCOPY
- AMINES
- THERMOGRAVIMETRIC ANALYSIS
- TOLUENES
- DIMERS
- SOLID STATE CHEMISTRY
- SULFUR
- WALLS
- CHEMICAL REACTIONS
- ETHYLENE
- SATURATION
- COOLING
- REFLECTION
- X RAY DIFFRACTION
- STRUCTURES
- CELLS
Subject Categories:
- Organic Chemistry
- Physical Chemistry
- Polymer Chemistry
- Atomic and Molecular Physics and Spectroscopy