In Situ Studies of the Formation of Tungsten and Niobium Oxide Nanoparticles: Towards Automated Analysis of Reaction Pathways from PDF Analysis using the Pearson Correlation Coefficient
Publikation: Bidrag til tidsskrift › Tidsskriftartikel › Forskning › fagfællebedømt
Standard
In Situ Studies of the Formation of Tungsten and Niobium Oxide Nanoparticles : Towards Automated Analysis of Reaction Pathways from PDF Analysis using the Pearson Correlation Coefficient. / Kjær, Emil T. S.; Aalling‐frederiksen, Olivia; Yang, Long; Thomas, Nancy K.; Juelsholt, Mikkel; Billinge, Simon J. L.; Jensen, Kirsten M. Ø.
I: Chemistry–Methods, Bind 2, Nr. 9, e202200034, 2022.Publikation: Bidrag til tidsskrift › Tidsskriftartikel › Forskning › fagfællebedømt
Harvard
APA
Vancouver
Author
Bibtex
}
RIS
TY - JOUR
T1 - In Situ Studies of the Formation of Tungsten and Niobium Oxide Nanoparticles
T2 - Towards Automated Analysis of Reaction Pathways from PDF Analysis using the Pearson Correlation Coefficient
AU - Kjær, Emil T. S.
AU - Aalling‐frederiksen, Olivia
AU - Yang, Long
AU - Thomas, Nancy K.
AU - Juelsholt, Mikkel
AU - Billinge, Simon J. L.
AU - Jensen, Kirsten M. Ø.
PY - 2022
Y1 - 2022
N2 - Using Pair Distribution Function (PDF) analysis of in situ total scattering data, we investigate the formation of tungsten and niobium oxides in a simple solvothermal synthesis. We use Pearson Correlation Coefficient (PCC) analysis of the time resolved PDFs to both map the structural changes taking place throughout the synthesis and identify structural models for precursor and product through PCC-based structure mining. Our analysis first shows that ultra-small tungsten and niobium oxide nanoparticles form instantaneously upon heating, with sizes between 1.5 and 2 nm. We show that the main structural motifs in the nanoparticles can be described with structures containing pentagonal columns, which is characteristic for many bulk tungsten and niobium oxides. We furthermore elucidate the structure of the precursor complex as clusters of octahedra with O- and Cl-ligands. The PCC based methodology automates the structure characterization and proves useful for analysis of large datasets of for example, time resolved X-ray scattering studies. The PCC is implemented in ‘PDF in the cloud’, a web platform for PDF analysis.
AB - Using Pair Distribution Function (PDF) analysis of in situ total scattering data, we investigate the formation of tungsten and niobium oxides in a simple solvothermal synthesis. We use Pearson Correlation Coefficient (PCC) analysis of the time resolved PDFs to both map the structural changes taking place throughout the synthesis and identify structural models for precursor and product through PCC-based structure mining. Our analysis first shows that ultra-small tungsten and niobium oxide nanoparticles form instantaneously upon heating, with sizes between 1.5 and 2 nm. We show that the main structural motifs in the nanoparticles can be described with structures containing pentagonal columns, which is characteristic for many bulk tungsten and niobium oxides. We furthermore elucidate the structure of the precursor complex as clusters of octahedra with O- and Cl-ligands. The PCC based methodology automates the structure characterization and proves useful for analysis of large datasets of for example, time resolved X-ray scattering studies. The PCC is implemented in ‘PDF in the cloud’, a web platform for PDF analysis.
U2 - 10.1002/cmtd.202200034
DO - 10.1002/cmtd.202200034
M3 - Journal article
VL - 2
JO - Chemistry–Methods
JF - Chemistry–Methods
SN - 2628-9725
IS - 9
M1 - e202200034
ER -
ID: 338529088