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Title: Cadmium amido alkoxide and alkoxide precursors for the synthesis of nanocrystalline CdE (E=S,Se, Te).

Abstract

The synthesis and characterization of a family of alternative precursors for the production of CdE nanoparticles (E = S, Se, and Te) is reported. The reaction of Cd(NR{sub 2}){sub 2} where NR{sub 2} = N(SiMe{sub 3}){sub 2} with n HOR led to the isolation of the following: n = 1 [Cd({mu}-OCH{sub 2}CMe{sub 3})(NR{sub 2})(py)]{sub 2} (1, py = pyridine), Cd[({mu}-OC{sub 6}H{sub 3}(Me){sub 2}-2,6){sub 2}Cd(NR{sub 2})(py)]{sub 2} (2), [Cd({mu}-OC{sub 6}H{sub 3}(CHMe{sub 2}){sub 2}-2,6)(NR{sub 2})(py)]{sub 2} (3), [Cd({mu}-OC{sub 6}H{sub 3}(CMe{sub 3}){sub 2}-2,6)(NR{sub 2})(py)]{sub 2} (4), [Cd({mu}-OC{sub 6}H{sub 2}(NH{sub 2}){sub 3}-2,4,6)(NR{sub 2})(py)]{sub 2} (5), and n = 2 [Cd({mu}-OC{sub 6}H{sub 3}(Me){sub 2}-2,6)(OC{sub 6}H{sub 3}(Me){sub 2}-2,6)(py){sub 2}]{sub 2} (6), and [Cd({mu}-OC{sub 6}H{sub 3}(CMe{sub 3}){sub 2}-2,6)(OC{sub 6}H{sub 3}(CMe{sub 3}){sub 2}-2,6)(THF)]{sub 2} (7). For all but 2, the X-ray crystal structures were solved as discrete dinuclear units bridged by alkoxide ligands and either terminal -NR{sub 2} or -OR ligands depending on the stoichiometry of the initial reaction. For 2, a trinuclear species was isolated using four {mu}-OR and two terminal -NR{sub 2} ligands. The coordination of the Cd metal center varied from 3 to 5 where the higher coordination numbers were achieved by binding Lewis basic solvents for the less sterically demanding ligands. These complexes weremore » further characterized in solution by {sup 1}H, {sup 13}C, and {sup 113}Cd NMR along with solid-state {sup 113}Cd NMR spectroscopy. The utility of these complexes as 'alternative precursors' for the controlled preparation of nanocrystalline CdS, CdSe, and CdTe was explored. To synthesize CdE nanocrystals, select species from this family of compounds were individually heated in a coordinating solvent (trioctylphosphine oxide) and then injected with the appropriate chalcogenide stock solution. Transmission electron spectroscopy and UV-vis spectroscopy were used to characterize the resultant particles.« less

Authors:
; ; ; ; ;
Publication Date:
Research Org.:
Sandia National Laboratories
Sponsoring Org.:
USDOE
OSTI Identifier:
952139
Report Number(s):
SAND2004-6554J
TRN: US200913%%384
DOE Contract Number:  
AC04-94AL85000
Resource Type:
Journal Article
Journal Name:
Proposed for publication in Chemistry of Materials.
Additional Journal Information:
Journal Name: Proposed for publication in Chemistry of Materials.
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; ALKOXIDES; CADMIUM; CHALCOGENIDES; COORDINATION NUMBER; CRYSTAL STRUCTURE; ELECTRON SPECTROSCOPY; PRODUCTION; PYRIDINE; SOLVENTS; SPECTROSCOPY; STOICHIOMETRY; SYNTHESIS

Citation Formats

Boyle, Timothy J., Avilucea, Gabriel, Bunge, Scott D., Alam, Todd Michael, Headley, Thomas Jeffrey, and Holland, Gregory P. Cadmium amido alkoxide and alkoxide precursors for the synthesis of nanocrystalline CdE (E=S,Se, Te).. United States: N. p., 2004. Web.
Boyle, Timothy J., Avilucea, Gabriel, Bunge, Scott D., Alam, Todd Michael, Headley, Thomas Jeffrey, & Holland, Gregory P. Cadmium amido alkoxide and alkoxide precursors for the synthesis of nanocrystalline CdE (E=S,Se, Te).. United States.
Boyle, Timothy J., Avilucea, Gabriel, Bunge, Scott D., Alam, Todd Michael, Headley, Thomas Jeffrey, and Holland, Gregory P. Wed . "Cadmium amido alkoxide and alkoxide precursors for the synthesis of nanocrystalline CdE (E=S,Se, Te).". United States.
@article{osti_952139,
title = {Cadmium amido alkoxide and alkoxide precursors for the synthesis of nanocrystalline CdE (E=S,Se, Te).},
author = {Boyle, Timothy J. and Avilucea, Gabriel and Bunge, Scott D. and Alam, Todd Michael and Headley, Thomas Jeffrey and Holland, Gregory P.},
abstractNote = {The synthesis and characterization of a family of alternative precursors for the production of CdE nanoparticles (E = S, Se, and Te) is reported. The reaction of Cd(NR{sub 2}){sub 2} where NR{sub 2} = N(SiMe{sub 3}){sub 2} with n HOR led to the isolation of the following: n = 1 [Cd({mu}-OCH{sub 2}CMe{sub 3})(NR{sub 2})(py)]{sub 2} (1, py = pyridine), Cd[({mu}-OC{sub 6}H{sub 3}(Me){sub 2}-2,6){sub 2}Cd(NR{sub 2})(py)]{sub 2} (2), [Cd({mu}-OC{sub 6}H{sub 3}(CHMe{sub 2}){sub 2}-2,6)(NR{sub 2})(py)]{sub 2} (3), [Cd({mu}-OC{sub 6}H{sub 3}(CMe{sub 3}){sub 2}-2,6)(NR{sub 2})(py)]{sub 2} (4), [Cd({mu}-OC{sub 6}H{sub 2}(NH{sub 2}){sub 3}-2,4,6)(NR{sub 2})(py)]{sub 2} (5), and n = 2 [Cd({mu}-OC{sub 6}H{sub 3}(Me){sub 2}-2,6)(OC{sub 6}H{sub 3}(Me){sub 2}-2,6)(py){sub 2}]{sub 2} (6), and [Cd({mu}-OC{sub 6}H{sub 3}(CMe{sub 3}){sub 2}-2,6)(OC{sub 6}H{sub 3}(CMe{sub 3}){sub 2}-2,6)(THF)]{sub 2} (7). For all but 2, the X-ray crystal structures were solved as discrete dinuclear units bridged by alkoxide ligands and either terminal -NR{sub 2} or -OR ligands depending on the stoichiometry of the initial reaction. For 2, a trinuclear species was isolated using four {mu}-OR and two terminal -NR{sub 2} ligands. The coordination of the Cd metal center varied from 3 to 5 where the higher coordination numbers were achieved by binding Lewis basic solvents for the less sterically demanding ligands. These complexes were further characterized in solution by {sup 1}H, {sup 13}C, and {sup 113}Cd NMR along with solid-state {sup 113}Cd NMR spectroscopy. The utility of these complexes as 'alternative precursors' for the controlled preparation of nanocrystalline CdS, CdSe, and CdTe was explored. To synthesize CdE nanocrystals, select species from this family of compounds were individually heated in a coordinating solvent (trioctylphosphine oxide) and then injected with the appropriate chalcogenide stock solution. Transmission electron spectroscopy and UV-vis spectroscopy were used to characterize the resultant particles.},
doi = {},
journal = {Proposed for publication in Chemistry of Materials.},
number = ,
volume = ,
place = {United States},
year = {2004},
month = {12}
}