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Title: Pushing data quality for laboratory pair distribution function experiments

Abstract

Over the past decade, some studies with laboratory pair distribution function (PDF) data emerged. Yet, limited Qmax or instrumental resolution impeded in-depth structural refinements. With more advanced detector technologies, the question arose how to design novel PDF equipment for laboratories that will allow decent PDF refinements over r = 1–70 Å. It is crucial to reflect the essential requirements, namely, monochromatic X-rays, suppression of air scattering, instrumental resolution, and overall measurement times. The result is a novel PDF setup based on a STOE STADI P powder diffractometer in transmission-/Debye-Scherrer geometry with monochromatic Ag Kα1 radiation, featuring a MYTHEN2 4K detector covering a Q range of 0.3–20.5 Å–1. PDF data are collected in a moving PDF mode within 6 h. Structural signatures of liquids can be satisfactorily resolved in the PDF as shown for the ionic liquid hmimPF6. The high instrumental resolution is mirrored in low qdamp values determined from LaB6 measurements. PDF data from a powder sample of ca. 7 nm TiO2 nanoparticles were successfully refined over up to 70 Å with goodness-of-fit values Rw < 0.22 (respectively Rw = 0.18 over 30 Å), thanks to the low background and high instrumental resolution, hereby enlarging the accessible r range bymore » several tens of Angstroms compared to previous laboratory PDF studies.« less

Authors:
 [1];  [1];  [2];  [2];  [2];  [1]
+ Show Author Affiliations
  1. Univ. Bayreuth (Germany)
  2. STOE & Cie GmbH, Darmstadt (Germany)
Publication Date:
Research Org.:
Argonne National Laboratory (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
Sponsoring Org.:
German Research Foundation (DFG); Bavarian Polymer Institute (BPI)
OSTI Identifier:
1512996
Grant/Contract Number:  
ZO 369/2-1
Resource Type:
Accepted Manuscript
Journal Name:
Review of Scientific Instruments
Additional Journal Information:
Journal Volume: 90; Journal Issue: 4; Journal ID: ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)
Country of Publication:
United States
Language:
ENGLISH
Subject:
47 OTHER INSTRUMENTATION; Scattering; Diffractometers; Ionic liquids; Powder diffraction; X-ray diffraction; Nanoparticles

Citation Formats

Thomae, Sabrina L. J., Prinz, Nils, Hartmann, Thomas, Teck, Michael, Correll, Sascha, and Zobel, Mirijam. Pushing data quality for laboratory pair distribution function experiments. United States: N. p., 2019. Web. doi:10.1063/1.5093714.
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Thomae, Sabrina L. J., Prinz, Nils, Hartmann, Thomas, Teck, Michael, Correll, Sascha, & Zobel, Mirijam. Pushing data quality for laboratory pair distribution function experiments. United States. https://doi.org/10.1063/1.5093714
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Thomae, Sabrina L. J., Prinz, Nils, Hartmann, Thomas, Teck, Michael, Correll, Sascha, and Zobel, Mirijam. Wed . "Pushing data quality for laboratory pair distribution function experiments". United States. https://doi.org/10.1063/1.5093714. https://www.osti.gov/servlets/purl/1512996.
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@article{osti_1512996,
title = {Pushing data quality for laboratory pair distribution function experiments},
author = {Thomae, Sabrina L. J. and Prinz, Nils and Hartmann, Thomas and Teck, Michael and Correll, Sascha and Zobel, Mirijam},
abstractNote = {Over the past decade, some studies with laboratory pair distribution function (PDF) data emerged. Yet, limited Qmax or instrumental resolution impeded in-depth structural refinements. With more advanced detector technologies, the question arose how to design novel PDF equipment for laboratories that will allow decent PDF refinements over r = 1–70 Å. It is crucial to reflect the essential requirements, namely, monochromatic X-rays, suppression of air scattering, instrumental resolution, and overall measurement times. The result is a novel PDF setup based on a STOE STADI P powder diffractometer in transmission-/Debye-Scherrer geometry with monochromatic Ag Kα1 radiation, featuring a MYTHEN2 4K detector covering a Q range of 0.3–20.5 Å–1. PDF data are collected in a moving PDF mode within 6 h. Structural signatures of liquids can be satisfactorily resolved in the PDF as shown for the ionic liquid hmimPF6. The high instrumental resolution is mirrored in low qdamp values determined from LaB6 measurements. PDF data from a powder sample of ca. 7 nm TiO2 nanoparticles were successfully refined over up to 70 Å with goodness-of-fit values Rw < 0.22 (respectively Rw = 0.18 over 30 Å), thanks to the low background and high instrumental resolution, hereby enlarging the accessible r range by several tens of Angstroms compared to previous laboratory PDF studies.},
doi = {10.1063/1.5093714},
journal = {Review of Scientific Instruments},
number = 4,
volume = 90,
place = {United States},
year = {Wed Apr 17 00:00:00 EDT 2019},
month = {Wed Apr 17 00:00:00 EDT 2019}
}
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https://doi.org/10.1063/1.5093714
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