Exploration of anion effects in solvothermal synthesis using in situ X-ray diffraction

Nils Lau Nyborg Broge, Andreas Dueholm Bertelsen, Ida Gjerlevsen Nielsen, Magnus Kløve, Martin Roelsgaard, Ann-Christin Dippel, Mads Ry Vogel Jørgensen, Bo Brummerstedt Iversen*

*Corresponding author for this work

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

Abstract

Solvothermal synthesis presents a facile and highly flexible approach to chemical processing and it is widely used for preparation of micro- and nanosized inorganic materials. The large number of synthesis parameters in combination with the richness of inorganic chemistry means that it is difficult to predict or design synthesis outcomes, and it is demanding to uncover the effect of different parameters due to the sealed and complex nature of solvothermal reactors along with the time demands related to reactor cleaning, sample purification, and characterization. This study explores the effect on formation of crystalline products of six common anions in solvothermal treatment of aqueous and ethanolic precursors. Three different cations are included in the study (Mn2+, Co2+, Cu2+) representing chemical affinities towards different regions of the periodic table with respect to the hard soft acid base (HSAB) classification and the Goldschmidt classification. They additionally belong to the commonly used 3d transition metals and display a suitable variety in solvothermal chemistry to highlight anion effects. The results of the solvothermal in situ experiments demonstrate a clear effect of the precursor anions, with respect to whether crystallization occurs or not and the characteristics of the formed phases. Additionally, some of the anions are shown to be redox active and to influence the formation temperature of certain phases which in turn relates to the observed average crystallite sizes.

Original languageEnglish
JournalPhysical Chemistry Chemical Physics
Volume26
Issue15
Pages (from-to)12121-12132
Number of pages12
DOIs
Publication statusPublished - Apr 2024

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