In situ X-ray diffraction study of the solvothermal formation mechanism of gallium oxide nanoparticles

Ida Gjerlevsen Nielsen, Magnus Kløve, Martin Roelsgaard, Ann Christin Dippel, Bo Brummerstedt Iversen*

*Corresponding author for this work

Research output: Contribution to journal/Conference contribution in journal/Contribution to newspaperJournal articleResearchpeer-review

Abstract

Gallium oxides are of broad interest due to their wide band gaps and attractive photoelectric properties. Typically, the synthesis of gallium oxide nanoparticles is based on a combination of solvent-based methods and subsequent calcination, but detailed information about solvent based formation processes is lacking, and this limits the tailoring of materials. Here we have examined the formation mechanisms and crystal structure transformations of gallium oxides during solvothermal synthesis using in situ X-ray diffraction. γ-Ga2O3 readily forms over a wide range of conditions. In contrast, β-Ga2O3 only forms at high temperatures (T > 300 °C), and it is always preceded by γ-Ga2O3, indicating that γ-Ga2O3 is a crucial part of the formation mechanism of β-Ga2O3. The activation energy for formation of β-Ga2O3 from γ-Ga2O3 is determined to be 90-100 kJ mol−1 in ethanol, water and aqueous NaOH based on kinetic modelling of phase fractions obtained from multi-temperature in situ X-ray diffraction data. At low temperatures GaOOH and Ga5O7OH form in aqueous solvent, but these phases are also obtained from γ-Ga2O3. Systematic exploration of synthesis parameters such as temperature, heating rate, solvent and reaction time reveal that they all affect the resulting product. In general, the solvent based reaction paths are different from reports on solid state calcination studies. This underlines that the solvent is an active part of the solvothermal reactions and to a high degree determines different formation mechanisms.

Original languageEnglish
JournalNanoscale
Volume15
Issue11
Pages (from-to)5284-5292
Number of pages9
ISSN2040-3364
DOIs
Publication statusPublished - Mar 2023

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