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Title: Synthesis and characterization of volatile bismuth [beta]-diketonate compounds for metal-organic chemical vapor deposition of thin films

Abstract

The synthesis of several new Bi(III) [beta]-diketonate complexes is described. In this method the chelates of the anions of 6,6,7,7.8,8,8-heptafluoro-2,2-dimethyl-3,5-octanedione (H(fod)) and 1,1,1,5,5,5-hexafluoro-2,4-pentanedione (H(hfa)) are formed by refluxing 3 equiv of the protonated ligand with 1 equiv of triphenylbismuth. The same reaction with 1,1,1-trifluoro-2,4-pentanedione (H(tfa)) produced a mixed [beta]-diketonate/phenyl ligand complex. The reaction products were characterized by thermogravimetric analysis, mass spectroscopy, nuclear magnetic resonance spectrometry, and gas chromatography/mass spectroscopy. Formation of bismuth-containing thin films using metal-organic chemical vapor deposition was demonstrated using the Bi(III) complex of fod. The films produced using this method were determined to contain 76% bismuth by Auger analysis, and no fluorine contamination was observed. 18 refs., 6 figs., 1 tab.

Authors:
 [1]; ; ;  [2]; ;  [3]
  1. Univ. of Illinois, Urbana, IL (United States)
  2. Univ. of Colorado, Boulder, CO (United States)
  3. SUNY, Albany, NY (United States)
OSTI Identifier:
7168046
Resource Type:
Journal Article
Journal Name:
Chemistry of Materials; (United States)
Additional Journal Information:
Journal Volume: 4:4; Journal ID: ISSN 0897-4756
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; BISMUTH; CHEMICAL VAPOR DEPOSITION; BISMUTH COMPLEXES; STRUCTURAL CHEMICAL ANALYSIS; AUGER ELECTRON SPECTROSCOPY; CHEMICAL PREPARATION; KETONES; MAGNETIC PROPERTIES; MASS SPECTROSCOPY; ORGANIC FLUORINE COMPOUNDS; THERMAL GRAVIMETRIC ANALYSIS; CHEMICAL ANALYSIS; CHEMICAL COATING; COMPLEXES; DEPOSITION; ELECTRON SPECTROSCOPY; ELEMENTS; GRAVIMETRIC ANALYSIS; METALS; ORGANIC COMPOUNDS; ORGANIC HALOGEN COMPOUNDS; PHYSICAL PROPERTIES; QUANTITATIVE CHEMICAL ANALYSIS; SPECTROSCOPY; SURFACE COATING; SYNTHESIS; THERMAL ANALYSIS; 360101* - Metals & Alloys- Preparation & Fabrication; 400201 - Chemical & Physicochemical Properties

Citation Formats

Brooks, K C, Turnipseed, S B, Barkley, R M, Sievers, R E, Tulchinsky, V, and Kaloyeros, A E. Synthesis and characterization of volatile bismuth [beta]-diketonate compounds for metal-organic chemical vapor deposition of thin films. United States: N. p., Web. doi:10.1021/cm00022a030.
Brooks, K C, Turnipseed, S B, Barkley, R M, Sievers, R E, Tulchinsky, V, & Kaloyeros, A E. Synthesis and characterization of volatile bismuth [beta]-diketonate compounds for metal-organic chemical vapor deposition of thin films. United States. https://doi.org/10.1021/cm00022a030
Brooks, K C, Turnipseed, S B, Barkley, R M, Sievers, R E, Tulchinsky, V, and Kaloyeros, A E. . "Synthesis and characterization of volatile bismuth [beta]-diketonate compounds for metal-organic chemical vapor deposition of thin films". United States. https://doi.org/10.1021/cm00022a030.
@article{osti_7168046,
title = {Synthesis and characterization of volatile bismuth [beta]-diketonate compounds for metal-organic chemical vapor deposition of thin films},
author = {Brooks, K C and Turnipseed, S B and Barkley, R M and Sievers, R E and Tulchinsky, V and Kaloyeros, A E},
abstractNote = {The synthesis of several new Bi(III) [beta]-diketonate complexes is described. In this method the chelates of the anions of 6,6,7,7.8,8,8-heptafluoro-2,2-dimethyl-3,5-octanedione (H(fod)) and 1,1,1,5,5,5-hexafluoro-2,4-pentanedione (H(hfa)) are formed by refluxing 3 equiv of the protonated ligand with 1 equiv of triphenylbismuth. The same reaction with 1,1,1-trifluoro-2,4-pentanedione (H(tfa)) produced a mixed [beta]-diketonate/phenyl ligand complex. The reaction products were characterized by thermogravimetric analysis, mass spectroscopy, nuclear magnetic resonance spectrometry, and gas chromatography/mass spectroscopy. Formation of bismuth-containing thin films using metal-organic chemical vapor deposition was demonstrated using the Bi(III) complex of fod. The films produced using this method were determined to contain 76% bismuth by Auger analysis, and no fluorine contamination was observed. 18 refs., 6 figs., 1 tab.},
doi = {10.1021/cm00022a030},
url = {https://www.osti.gov/biblio/7168046}, journal = {Chemistry of Materials; (United States)},
issn = {0897-4756},
number = ,
volume = 4:4,
place = {United States},
year = {},
month = {}
}