TY  - JOUR
AU  - Juelsholt, Mikkel
AU  - Aalling-Frederiksen, Olivia
AU  - Lindahl Christiansen, Troels
AU  - Kjær, Emil T. S.
AU  - Lefeld, Niels
AU  - Kirsch, Andrea
AU  - Jensen, Kirsten Marie
TI  - Influence of the Precursor Structure on the Formation of Tungsten Oxide Polymorphs
JO  - Inorganic chemistry
VL  - 62
IS  - 37
SN  - 0020-1669
CY  - Washington, DC
PB  - American Chemical Society
M1  - PUBDB-2024-00208
SP  - 14949 - 14958
PY  - 2023
AB  - Understanding material nucleation processes is crucial for the development of synthesis pathways for tailormade materials. However, we currently have little knowledge of the influence of the precursor solution structure on the formation pathway of materials. We here use in situ total scattering to show how the precursor solution structure influences which crystal structure is formed during the hydrothermal synthesis of tungsten oxides. We investigate the synthesis of tungsten oxide from the two polyoxometalate salts, ammonium metatungstate, and ammonium paratungstate. In both cases, a hexagonal ammonium tungsten bronze (NH<sub>4</sub>)<sub>0.25</sub>WO<sub>3</sub> is formed as the final product. If the precursor solution contains metatungstate clusters, this phase forms directly in the hydrothermal synthesis. However, if the paratungstate B cluster is present at the time of crystallization, a metastable intermediate phase in the form of a pyrochlore-type tungsten oxide, WO<sub>3</sub>·0.5H<sub>2</sub>O, initially forms. The pyrochlore structure then undergoes a phase transformation into the tungsten bronze phase. Our studies thus experimentally show that the precursor cluster structure present at the moment of crystallization directly influences the formed crystalline phase and suggests that the precursor structure just prior to crystallization can be used as a tool for targeting specific crystalline phases of interest.
LB  - PUB:(DE-HGF)16
C6  - 37658472
UR  - <Go to ISI:>//WOS:001122051400001
DO  - DOI:10.1021/acs.inorgchem.3c01659
UR  - https://bib-pubdb1.desy.de/record/601478
ER  -