Solvothermal synthesis of ultrasmall tungsten oxide nanoparticles
The synthesis of catalytically useful, ultrasmall oxide nanoparticles (NPs) of group 5 and 6 metals is not readily achievable through reported methods. In this work, we introduce a one-pot, two-precursor synthesis route to <2 nm MO(x) NPs in which a polyoxometalate salt is decomposed thermally in...
| Veröffentlicht in: | Langmuir : the ACS journal of surfaces and colloids. - 1992. - 28(2012), 51 vom: 21. Dez., Seite 17771-7 |
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| Weitere Verfasser: | , , |
| Format: | Online-Aufsatz |
| Sprache: | English |
| Veröffentlicht: |
2012
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| Zugriff auf das übergeordnete Werk: | Langmuir : the ACS journal of surfaces and colloids |
| Schlagworte: | Journal Article |
| Zusammenfassung: | The synthesis of catalytically useful, ultrasmall oxide nanoparticles (NPs) of group 5 and 6 metals is not readily achievable through reported methods. In this work, we introduce a one-pot, two-precursor synthesis route to <2 nm MO(x) NPs in which a polyoxometalate salt is decomposed thermally in a high-boiling organic solvent oleylamine. The use of ammonium metatungstate resulted in oleylamine-coated, crystalline WO(x) NPs at consistently high yields of 92 ± 5%. The semicrystalline NPs contained 20-36 WO(x) structural units per particle, as determined from aberration-corrected high-resolution scanning transmission electron microscopy, and an organic coating of 16-20 oleylamine molecules, as determined by thermogravimetric analysis. The NPs had a mean size of 1.6 ± 0.3 nm, as estimated from atomic force microscopy and small-angle X-ray scattering measurements. Carrying out the synthesis in the presence of organic oxidant trimethylamine N-oxide led to smaller WO(x) NPs (1.0 ± 0.4 nm), whereas the reductant 1,12-dodecanediol led to WO(x) nanorods (4 ± 1 nm × 20 ± 5 nm). These findings provide a new method to control the size and shape of transition metal oxide NPs, which will be especially useful in catalysis |
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| Beschreibung: | Date Completed 23.05.2013 Date Revised 21.12.2012 published: Print-Electronic Citation Status PubMed-not-MEDLINE |
| ISSN: | 1520-5827 |
| DOI: | 10.1021/la3029462 |