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):

• Hampden-Smith, Mark J.
• Zeng, D.
• Datye, A.
• Powell, Q.
• Gurav, A.

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

Distribution Statement:

APPROVED FOR PUBLIC RELEASE