A new method for in situ structural investigations of nano-sized amorphous and crystalline materials using mixed-flow reactors
Abstract
Structural investigations of amorphous and nanocrystalline phases forming in solution are historically challenging. Few methods are capable of in situ atomic structural analysis and rigorous control of the system. A mixed-flow reactor (MFR) is used for total X-ray scattering experiments to examine the short- and long-range structure of phases in situ with pair distribution function (PDF) analysis. The adaptable experimental setup enables data collection for a range of different system chemistries, initial supersaturations and residence times. The age of the sample during analysis is controlled by adjusting the flow rate. Faster rates allow for younger samples to be examined, but if flow is too fast not enough data are acquired to average out excess signal noise. Slower flow rates form older samples, but at very slow speeds particles settle and block flow, clogging the system. Proper background collection and subtraction is critical for data optimization. Overall, this MFR method is an ideal scheme for analyzing the in situ structures of phases that form during crystal growth in solution. As a proof of concept, high-resolution total X-ray scattering data of amorphous and crystalline calcium phosphates and amorphous calcium carbonate were collected for PDF analysis.
- Publication Date:
- Research Org.:
- Argonne National Lab. (ANL), Argonne, IL (United States)
- Sponsoring Org.:
- USDOE Office of Science (SC), Basic Energy Sciences (BES)
- OSTI Identifier:
- 1617945
- Alternate Identifier(s):
- OSTI ID: 1575251
- Grant/Contract Number:
- BES-FG02-00ER15112; AC02-06CH11357
- Resource Type:
- Published Article
- Journal Name:
- Acta Crystallographica. Section A, Foundations and Advances (Online)
- Additional Journal Information:
- Journal Name: Acta Crystallographica. Section A, Foundations and Advances (Online) Journal Volume: 75 Journal Issue: 5; Journal ID: ISSN 2053-2733
- Publisher:
- International Union of Crystallography (IUCr)
- Country of Publication:
- Denmark
- Language:
- English
- Subject:
- 36 MATERIALS SCIENCE; in situ X-ray total scattering; crystallization; amorphous calcium phosphate; amorphous calcium carbonate; pair distribution function analysis
Citation Formats
Hoeher, Alexandria, Mergelsberg, Sebastian, Borkiewicz, Olaf J., Dove, Patricia M., and Michel, F. Marc. A new method for in situ structural investigations of nano-sized amorphous and crystalline materials using mixed-flow reactors. Denmark: N. p., 2019.
Web. doi:10.1107/S2053273319008623.
Hoeher, Alexandria, Mergelsberg, Sebastian, Borkiewicz, Olaf J., Dove, Patricia M., & Michel, F. Marc. A new method for in situ structural investigations of nano-sized amorphous and crystalline materials using mixed-flow reactors. Denmark. https://doi.org/10.1107/S2053273319008623
Hoeher, Alexandria, Mergelsberg, Sebastian, Borkiewicz, Olaf J., Dove, Patricia M., and Michel, F. Marc. Fri .
"A new method for in situ structural investigations of nano-sized amorphous and crystalline materials using mixed-flow reactors". Denmark. https://doi.org/10.1107/S2053273319008623.
@article{osti_1617945,
title = {A new method for in situ structural investigations of nano-sized amorphous and crystalline materials using mixed-flow reactors},
author = {Hoeher, Alexandria and Mergelsberg, Sebastian and Borkiewicz, Olaf J. and Dove, Patricia M. and Michel, F. Marc},
abstractNote = {Structural investigations of amorphous and nanocrystalline phases forming in solution are historically challenging. Few methods are capable of in situ atomic structural analysis and rigorous control of the system. A mixed-flow reactor (MFR) is used for total X-ray scattering experiments to examine the short- and long-range structure of phases in situ with pair distribution function (PDF) analysis. The adaptable experimental setup enables data collection for a range of different system chemistries, initial supersaturations and residence times. The age of the sample during analysis is controlled by adjusting the flow rate. Faster rates allow for younger samples to be examined, but if flow is too fast not enough data are acquired to average out excess signal noise. Slower flow rates form older samples, but at very slow speeds particles settle and block flow, clogging the system. Proper background collection and subtraction is critical for data optimization. Overall, this MFR method is an ideal scheme for analyzing the in situ structures of phases that form during crystal growth in solution. As a proof of concept, high-resolution total X-ray scattering data of amorphous and crystalline calcium phosphates and amorphous calcium carbonate were collected for PDF analysis.},
doi = {10.1107/S2053273319008623},
journal = {Acta Crystallographica. Section A, Foundations and Advances (Online)},
number = 5,
volume = 75,
place = {Denmark},
year = {2019},
month = {8}
}
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https://doi.org/10.1107/S2053273319008623
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