Journal
ACS APPLIED ENERGY MATERIALS
Volume 4, Issue 1, Pages 42-46Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acsaem.0c02996
Keywords
iron chalcogenide; solvothermal synthesis; intercalation; crystal structure; in situ
Funding
- National Science Foundation [DMR-2003783]
- U.S. DOE [DE-AC02-06CH11357]
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Two solvothermal pathways were reported for the preparation of intercalated iron sulfide [Fe8S10]Fe(en)(3)·en(0.5), showing that diamines can intercalate as charged coordination complexes in layered iron chalcogenides along with neutral diamine molecules.
We report two solvothermal pathways toward intercalated iron sulfide, [Fe8S10]Fe(en)(3)center dot en(0.5) (en = ethylenediamine), featuring [Fe8S11](2-) layers stacked by [Fe(en)(3)](2+) cations and free ethylenediamine molecules. [Fe8S10]Fe(en)(3)center dot en(0.5) is synthesized in a simple single-step method from Fe and S in ethylenediamine with addition of NH4Cl mineralizer as well as from solvothermal treatment of mackinawite, tetragonal FeS. In situ synchrotron powder X-ray diffraction experiments reveal a clear transformation of tetragonal FeS into [Fe8S10]Fe(en)(3)center dot en(0.5) upon reaction with ethylenediamine. In-house control synthetic experiments confirmed the chemical process, whereby ethylenediamine leaches iron solely from the tetragonal Fe-S layers to form [Fe(en)(3)](2+) complexes and thereby oxidize the intralayer iron to Fe2.25+. Our report emphasizes that, in layered iron chalcogenides, diamines can intercalate as charged coordination complexes in tandem with neutral diamine molecules.
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