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Title: New metal-organic chemistry of barium, an aqueous synthesis for volatile alkaline earth complexes, and synthesis and characterization of Tl-Ba-Ca-Cu-O thin films by metal-organic chemical vapor deposition

Abstract

The synthesis and characterization of six fluorine-free Barium MOCVD (metal-organic chemical vapor deposition) precursors based upon encapsulating [beta]-ketoiminate-polyether ligation and having the general formula Ba(RCOCHC (NR[prime])R[prime])2 (R[prime] = [sup t]butyl, R[prime] = polyether, and R[double prime] = methyl or [sup t]butyl) is reported. The complexes were prepared by a nonaqueous approach which employs BaH[sub 2] and the corresponding [beta]-ketoimine. These complexes have been characterized by [sup 1]H and [sup 13]C NMR spectroscopy, elemental analysis, mass spectroscopy, cryoscopic molecular weight determination, thermogravimetric analysis, and single crystal X-ray structural analysis. These complexes serve as volatile barium MOCVD precursors. BaPbO[sub 3] films have been grown using the barium [beta]-ketoiminate complexes and Pb(dipivaloylmethanate)[sub 2] as the barium and lead sources, and have been characterized. Investigation of thermolytic decomposition of the barium [beta]-ketoiminate complexes led to identification of 2-methyl-4-[sup 4]butylpyridine (17), pinacolone, and 2,2-dimethyl-5-imino-3-hexanone as the major organic thermolysis products of 11, 12, and 13. The MOVCD synthesis of Tl-Ba-Ca-Cu-O thin films on novel substrates has been investigated. These films were prepared in three steps: deposition of Ba-Ca-Cu-O-(F) thin films by MOCVD; defluorination via water/oxygen anneal; thallination using volatile thallium oxides. Films were characterized by X-ray diffraction, variable temperature magnetization, variable temperature conductivity, and scanningmore » and transmission electron microscopy. Attempts at preparing Tl-Ba-Ca-Cu-O thin films on Pt resulted in formation of a non-contiguous Ba-Ca-Cu-O film. Tl[sub 2]Ba[sub 2]Ca[sub 1]Cu[sub 2]O[sub x] on Au/YSZ, Au, and LaAlO[sub 3] show preferential orientation of crystallite c-axes. Au-Cu alloy formation was confirmed by TEM/EDS for Tl[sub 2]Ba[sub 2]Ca[sub 1]Cu[sub 2]O[sub x] thin films on Au.« less

Authors:
Publication Date:
Research Org.:
Northwestern Univ., Chicago, IL (United States)
OSTI Identifier:
7072311
Resource Type:
Miscellaneous
Resource Relation:
Other Information: Thesis (Ph.D.)
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; ALKALINE EARTH METAL COMPLEXES; CHEMICAL VAPOR DEPOSITION; BARIUM OXIDES; PRECURSOR; CALCIUM OXIDES; CUPRATES; INTERMETALLIC COMPOUNDS; ORGANOMETALLIC COMPOUNDS; THALLIUM OXIDES; THIN FILMS; ALKALINE EARTH METAL COMPOUNDS; ALLOYS; BARIUM COMPOUNDS; CALCIUM COMPOUNDS; CHALCOGENIDES; CHEMICAL COATING; COMPLEXES; COPPER COMPOUNDS; DEPOSITION; FILMS; ORGANIC COMPOUNDS; OXIDES; OXYGEN COMPOUNDS; SURFACE COATING; THALLIUM COMPOUNDS; TRANSITION ELEMENT COMPOUNDS; 360201* - Ceramics, Cermets, & Refractories- Preparation & Fabrication; 400201 - Chemical & Physicochemical Properties

Citation Formats

Schulz, D L. New metal-organic chemistry of barium, an aqueous synthesis for volatile alkaline earth complexes, and synthesis and characterization of Tl-Ba-Ca-Cu-O thin films by metal-organic chemical vapor deposition. United States: N. p., 1993. Web.
Schulz, D L. New metal-organic chemistry of barium, an aqueous synthesis for volatile alkaline earth complexes, and synthesis and characterization of Tl-Ba-Ca-Cu-O thin films by metal-organic chemical vapor deposition. United States.
Schulz, D L. Fri . "New metal-organic chemistry of barium, an aqueous synthesis for volatile alkaline earth complexes, and synthesis and characterization of Tl-Ba-Ca-Cu-O thin films by metal-organic chemical vapor deposition". United States.
@article{osti_7072311,
title = {New metal-organic chemistry of barium, an aqueous synthesis for volatile alkaline earth complexes, and synthesis and characterization of Tl-Ba-Ca-Cu-O thin films by metal-organic chemical vapor deposition},
author = {Schulz, D L},
abstractNote = {The synthesis and characterization of six fluorine-free Barium MOCVD (metal-organic chemical vapor deposition) precursors based upon encapsulating [beta]-ketoiminate-polyether ligation and having the general formula Ba(RCOCHC (NR[prime])R[prime])2 (R[prime] = [sup t]butyl, R[prime] = polyether, and R[double prime] = methyl or [sup t]butyl) is reported. The complexes were prepared by a nonaqueous approach which employs BaH[sub 2] and the corresponding [beta]-ketoimine. These complexes have been characterized by [sup 1]H and [sup 13]C NMR spectroscopy, elemental analysis, mass spectroscopy, cryoscopic molecular weight determination, thermogravimetric analysis, and single crystal X-ray structural analysis. These complexes serve as volatile barium MOCVD precursors. BaPbO[sub 3] films have been grown using the barium [beta]-ketoiminate complexes and Pb(dipivaloylmethanate)[sub 2] as the barium and lead sources, and have been characterized. Investigation of thermolytic decomposition of the barium [beta]-ketoiminate complexes led to identification of 2-methyl-4-[sup 4]butylpyridine (17), pinacolone, and 2,2-dimethyl-5-imino-3-hexanone as the major organic thermolysis products of 11, 12, and 13. The MOVCD synthesis of Tl-Ba-Ca-Cu-O thin films on novel substrates has been investigated. These films were prepared in three steps: deposition of Ba-Ca-Cu-O-(F) thin films by MOCVD; defluorination via water/oxygen anneal; thallination using volatile thallium oxides. Films were characterized by X-ray diffraction, variable temperature magnetization, variable temperature conductivity, and scanning and transmission electron microscopy. Attempts at preparing Tl-Ba-Ca-Cu-O thin films on Pt resulted in formation of a non-contiguous Ba-Ca-Cu-O film. Tl[sub 2]Ba[sub 2]Ca[sub 1]Cu[sub 2]O[sub x] on Au/YSZ, Au, and LaAlO[sub 3] show preferential orientation of crystallite c-axes. Au-Cu alloy formation was confirmed by TEM/EDS for Tl[sub 2]Ba[sub 2]Ca[sub 1]Cu[sub 2]O[sub x] thin films on Au.},
doi = {},
url = {https://www.osti.gov/biblio/7072311}, journal = {},
number = ,
volume = ,
place = {United States},
year = {1993},
month = {1}
}

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