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Title: In situ Synthesis of Mixed-Valent Manganese Oxide Nanocrystals: An In situ Synchrotron X-ray Diffraction Study

Abstract

Phase transformations of materials can be studied by in situ synchrotron X-ray diffraction. However, most reported in situ synchrotron XRD studies focus on solid state/gel systems by measuring phase/structure changes during application of pressure or heat. Phase transformations during material synthesis and their applications, especially in wet chemistry processes with different media, have not drawn much attention. Here, using manganese oxides as examples, we report the successful characterization of phase transformations in in situ hydrothermal synthesis conditions by the in situ synchrotron XRD method using a quartz/sapphire capillary tube as the synthesis reactor. The results were used for better design of materials with controlled structures and properties. This method can be generally used for synthesis of manganese oxides as well as for in situ characterization of other material syntheses using hydrothermal, sol-gel, and other methods. In addition, catalytic processes in liquid-solid, gas-solid, and solid-solid systems can also be studied in such an in situ way so that catalytic mechanisms can be better understood and catalyst synthesis and catalytic processes can be optimized.

Authors:
; ; ; ;
Publication Date:
Research Org.:
Brookhaven National Laboratory (BNL) National Synchrotron Light Source
Sponsoring Org.:
Doe - Office Of Science
OSTI Identifier:
914061
Report Number(s):
BNL-78629-2007-JA
Journal ID: ISSN 0002-7863; JACSAT; TRN: US0801510
DOE Contract Number:
DE-AC02-98CH10886
Resource Type:
Journal Article
Resource Relation:
Journal Name: J. Am. Chem. Soc.; Journal Volume: 128; Journal Issue: 14
Country of Publication:
United States
Language:
English
Subject:
43 PARTICLE ACCELERATORS; CATALYSTS; CHEMISTRY; DESIGN; HYDROTHERMAL SYNTHESIS; MANGANESE OXIDES; PHASE TRANSFORMATIONS; SYNCHROTRONS; SYNTHESIS; X-RAY DIFFRACTION; NSLS; national synchrotron light source

Citation Formats

Shen,X., Ding, Y., Hanson, J., Aindow, M., and Suib, S. In situ Synthesis of Mixed-Valent Manganese Oxide Nanocrystals: An In situ Synchrotron X-ray Diffraction Study. United States: N. p., 2006. Web. doi:10.1021/ja058456+.
Shen,X., Ding, Y., Hanson, J., Aindow, M., & Suib, S. In situ Synthesis of Mixed-Valent Manganese Oxide Nanocrystals: An In situ Synchrotron X-ray Diffraction Study. United States. doi:10.1021/ja058456+.
Shen,X., Ding, Y., Hanson, J., Aindow, M., and Suib, S. Sun . "In situ Synthesis of Mixed-Valent Manganese Oxide Nanocrystals: An In situ Synchrotron X-ray Diffraction Study". United States. doi:10.1021/ja058456+.
@article{osti_914061,
title = {In situ Synthesis of Mixed-Valent Manganese Oxide Nanocrystals: An In situ Synchrotron X-ray Diffraction Study},
author = {Shen,X. and Ding, Y. and Hanson, J. and Aindow, M. and Suib, S.},
abstractNote = {Phase transformations of materials can be studied by in situ synchrotron X-ray diffraction. However, most reported in situ synchrotron XRD studies focus on solid state/gel systems by measuring phase/structure changes during application of pressure or heat. Phase transformations during material synthesis and their applications, especially in wet chemistry processes with different media, have not drawn much attention. Here, using manganese oxides as examples, we report the successful characterization of phase transformations in in situ hydrothermal synthesis conditions by the in situ synchrotron XRD method using a quartz/sapphire capillary tube as the synthesis reactor. The results were used for better design of materials with controlled structures and properties. This method can be generally used for synthesis of manganese oxides as well as for in situ characterization of other material syntheses using hydrothermal, sol-gel, and other methods. In addition, catalytic processes in liquid-solid, gas-solid, and solid-solid systems can also be studied in such an in situ way so that catalytic mechanisms can be better understood and catalyst synthesis and catalytic processes can be optimized.},
doi = {10.1021/ja058456+},
journal = {J. Am. Chem. Soc.},
number = 14,
volume = 128,
place = {United States},
year = {Sun Jan 01 00:00:00 EST 2006},
month = {Sun Jan 01 00:00:00 EST 2006}
}