Method for continuous synthesis of metal oxide powders
Abstract
A method for the rapid and continuous production of crystalline mixed-metal oxides from a precursor solution comprised of a polymerizing agent, chelated metal ions, and a solvent. The method discharges solution droplets of less than 500 .mu.m diameter using an atomizing or spray-type process into a reactor having multiple temperature zones. Rapid evaporation occurs in a first zone, followed by mixed-metal organic foam formation in a second zone, followed by amorphous and partially crystalline oxide precursor formation in a third zone, followed by formation of the substantially crystalline mixed-metal oxide in a fourth zone. The method operates in a continuous rather than batch manner and the use of small droplets as the starting material for the temperature-based process allows relatively high temperature processing. In a particular embodiment, the first zone operates at 100-300.degree. C., the second zone operates at 300-700.degree. C., and the third operates at 700-1000.degree. C., and fourth zone operates at at least 700.degree. C. The resulting crystalline mixed-metal oxides display a high degree of crystallinity and sphericity with typical diameters on the order of 50 .mu.m or less.
- Inventors:
- Issue Date:
- Research Org.:
- National Energy Technology Laboratory (NETL), Pittsburgh, PA, Morgantown, WV (United States)
- Sponsoring Org.:
- USDOE
- OSTI Identifier:
- 1214149
- Patent Number(s):
- 9126833
- Application Number:
- 14/296,643
- Assignee:
- U.S. Department of Energy (Washington, DC)
- Patent Classifications (CPCs):
-
C - CHEMISTRY C01 - INORGANIC CHEMISTRY C01B - NON-METALLIC ELEMENTS
C - CHEMISTRY C01 - INORGANIC CHEMISTRY C01P - INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- Resource Type:
- Patent
- Resource Relation:
- Patent File Date: 2014 Jun 05
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 36 MATERIALS SCIENCE
Citation Formats
Berry, David A., Haynes, Daniel J., Shekhawat, Dushyant, and Smith, Mark W. Method for continuous synthesis of metal oxide powders. United States: N. p., 2015.
Web.
Berry, David A., Haynes, Daniel J., Shekhawat, Dushyant, & Smith, Mark W. Method for continuous synthesis of metal oxide powders. United States.
Berry, David A., Haynes, Daniel J., Shekhawat, Dushyant, and Smith, Mark W. Tue .
"Method for continuous synthesis of metal oxide powders". United States. https://www.osti.gov/servlets/purl/1214149.
@article{osti_1214149,
title = {Method for continuous synthesis of metal oxide powders},
author = {Berry, David A. and Haynes, Daniel J. and Shekhawat, Dushyant and Smith, Mark W.},
abstractNote = {A method for the rapid and continuous production of crystalline mixed-metal oxides from a precursor solution comprised of a polymerizing agent, chelated metal ions, and a solvent. The method discharges solution droplets of less than 500 .mu.m diameter using an atomizing or spray-type process into a reactor having multiple temperature zones. Rapid evaporation occurs in a first zone, followed by mixed-metal organic foam formation in a second zone, followed by amorphous and partially crystalline oxide precursor formation in a third zone, followed by formation of the substantially crystalline mixed-metal oxide in a fourth zone. The method operates in a continuous rather than batch manner and the use of small droplets as the starting material for the temperature-based process allows relatively high temperature processing. In a particular embodiment, the first zone operates at 100-300.degree. C., the second zone operates at 300-700.degree. C., and the third operates at 700-1000.degree. C., and fourth zone operates at at least 700.degree. C. The resulting crystalline mixed-metal oxides display a high degree of crystallinity and sphericity with typical diameters on the order of 50 .mu.m or less.},
doi = {},
journal = {},
number = ,
volume = ,
place = {United States},
year = {2015},
month = {9}
}
Works referenced in this record:
Method of Preparing Lead and Alkaline Earth Titanates and Niobates and Coating Method Using the Same to Form a Capacitor
patent, July 1967
- Pechini, Maggio P.
- US Patent Document 3,330,697
Processes for preparing mixed metal oxide powders
patent, November 2002
- Gulgun, Mehmet Ali; Kriven, Waltraud M.; Nguyen, My Hoang
- US Patent Document 6,482,387
Method for producing superconducting oxide compounds
patent, May 2003
- Kirkwood, Brad L.; Luhman, Thomas S.; Stephenson, Ronald R.
- US Patent Document 6,559,103
Mixed-metal oxide particles by liquid feed flame spray pyrolysis of oxide precursors in oxygenated solvents
patent, May 2007
- Sutorik, Anthony C.; Laine, Richard M.; Marchal, Julien
- US Patent Document 7,220,398
Method for producing cerium dioxide nanopowder by flame spray pyrolysis and cerium dioxide nanopowder produced by the method
patent, May 2012
- Chang, Han Kwon; Jang, Hee Dong; Kil, Dae Sup
- US Patent Document 8,187,562
Influence of Microwave-Assisted Pechini Method on La0.80Sr0.20Ga0.83Mg0.17O3-δ Ionic Conductivity
journal, January 2012
- Boldrini, S.; Mortalò, C.; Fasolin, S.
- Fuel Cells, Vol. 12, Issue 1
Controlling Microstructural Evolution in Pechini Gels through the Interplay between Precursor Complexation, Step-Growth Polymerization, and Template Confinement
journal, January 2013
- Rudisill, Stephen G.; Hein, Nicholas M.; Terzic, Denis
- Chemistry of Materials, Vol. 25, Issue 5