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Superconducting iron-selenide layered systems by hydrothermal syntheses

Subject Area Solid State and Surface Chemistry, Material Synthesis
Physical Chemistry of Solids and Surfaces, Material Characterisation
Term from 2015 to 2023
Project identifier Deutsche Forschungsgemeinschaft (DFG) - Project number 271160910
 
Final Report Year 2024

Final Report Abstract

In our project on iron-based superconducting materials, we made a series of discoveries that provide new insights into superconducting substances and the interactions between superconductivity, magnetism, and crystal structure. At the beginning of the funding period, we discovered the compound [(Li0.8Fe0.2)OH]FeSe, which is both superconducting (up to 42 K) and ferromagnetic (up to 10 K) - a unique phenomenon. We successfully grew millimeter-sized crystals and also synthesized the sulfur counterpart [(Li0.8Fe0.2)OH]FeS, as well as the series [(Li0.8Fe0.2)OH]FeSe1-xSx. Even small amounts of sulfur suppress superconductivity while preserving the magnetic properties. Further investigations of [(Li0.8Fe0.2)OH]FeSe revealed two superconducting states (at 40 K and 35 K) and confirmed the coexistence of superconductivity and magnetism. Surprisingly, hydrothermally synthesized β-FeSe is not superconducting. X-ray structural analysis at low temperatures showed the formation of a different crystal structure, in which the distances between the iron atoms differ, potentially explaining the absence of superconductivity. The hydrothermal synthesis method was also used for iron sulfide (FeS), which is superconducting at 4 K. Unlike FeSe, FeS shows no structural changes upon cooling, and its superconductivity disappears under pressure. Experiments on the hydrothermal synthesis of FeSe intercalation compounds led to the discovery of the compound [Na6(H2O)18][Fe4Se8], with iron atoms fluctuating between the Fe3+ and Fe2+ states. The crystal structure contains [(Fe4Se4)Se4]6- clusters surrounded exclusively by H2O molecules. In collaboration with our partners, we studied the magnetism of the mixedvalence clusters using µSR measurements. The results show that the fluctuation frequency decreases with decreasing temperature; however, the expected ground state with S = 0 was surprisingly not achieved. Further hydrothermal syntheses during the second funding period yielded mixed results, while solvothermal methods using ethylenediamine were more successful. We succeeded in intercalating neutral molecules into FeSe, but these compounds were not superconducting. Presumably, charge transfer is necessary to achieve high transition temperatures. Later in the project, we achieved the electrochemical intercalation of tetramethylammonium (TMA) into FeSe. (TMA)0.5Fe2Se2 is a new superconducting material with a transition temperature of 42 K. In the series (TMA)0.5Fe2Se2-xSx, the transition temperature decreases with increasing sulfur content. In collaboration with partners, we investigated the interplay of superconductivity, magnetism, and nematicity in FeSe1-xSx. Under pressure, all three phenomena could coexist, raising new questions about their significance for superconductivity.

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