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000644506 1001_ $$0P:(DE-H253)PIP1085597$$aZito, Cecilia A.$$b0
000644506 245__ $$aIn situ X-ray Synchrotron Studies Reveal the Nucleation and Topotactic Transformation of Iron Sulfide Nanosheets
000644506 260__ $$aWashington, DC$$bACS Publications$$c2025
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000644506 500__ $$aEuropean Research Council (ERC) LINCHPIN (grant no. 818941), the Deutsche Forschungsgemeinschaft (DFG) through the Cluster of Excellence “Advanced Imaging of Matter” (EXC 2056, project ID 390715994) and the Graduate School “Nanohybrid” (funding ID 408076438), and the Bundesministerium für Bildung und Forschung (BMBF) via the project 05K22GU7 (LUCENT II)
000644506 520__ $$aIron sulfides (FexSy), including greigite (Fe$_3$S$_4$), are key materials in geological processes and technological applications. However, in the context of colloidal synthesis, the mechanism by which these nanoparticles form remains unexplored. Here, we employ in situ X-ray diffraction and photon-in photon-out spectroscopic studies to elucidate the reaction pathway of Fe(acac)$_3$ and thioacetamide (TAA) in benzyl alcohol (BA), which yields crumpled Fe$_3$S$_4$ nanosheets. Using powder X-ray diffraction (PXRD), we identify FeS (mackinawite) as a crystalline intermediate whose anisotropic growth, driven by its layered crystal structure, governs the crumpled nanosheet-like morphology of Fe$_3$S$_4$ (greigite) through a topotactic transition. By performing high-resolution fluorescence-detected X-ray absorption near-edge structure (HERFD-XANES) spectroscopy, we show that the formation of Fe$_3$S$_4$ proceeds through a multistep mechanism involving two intermediates. Supported by density functional theory (DFT), we find that Fe(acac)$_3$ is initially reduced in the presence of TAA in BA, forming a molecular intermediate [Fe(acac)$_2$(BA)$_2$], which subsequently transforms into FeS and ultimately into Fe$_3$S$_4$. Complementary valence-to-core X-ray emission spectroscopy (vtc-XES) reveals the evolution of the coordination environment from Fe–O to Fe–S throughout the reaction. Our work provides a comprehensive understanding of the formation mechanism of Fe$_3$S$_4$ nanosheets in solution, shedding light on how crystal growth dynamics and electronic structure evolution dictate their unique crumpled nanosheet morphology.
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000644506 7001_ $$0P:(DE-H253)PIP1083268$$aKlemeyer, Lars$$b1
000644506 7001_ $$0P:(DE-H253)PIP1092080$$aCaddeo, Francesco$$b2
000644506 7001_ $$0P:(DE-H253)PIP1090769$$aJessen, Brian$$b3
000644506 7001_ $$0P:(DE-H253)PIP1083208$$aHarouna-Mayer, Sani Y.$$b4
000644506 7001_ $$00000-0003-3351-7949$$aLacroix, Lise-Marie$$b5
000644506 7001_ $$aLangfeldt, Malte$$b6
000644506 7001_ $$0P:(DE-H253)PIP1098796$$aGröne, Tjark L. R.$$b7
000644506 7001_ $$0P:(DE-H253)PIP1085745$$aKesavan, Jagadesh K.$$b8
000644506 7001_ $$0P:(DE-H253)PIP1092945$$aHsu, Chia-Shuo$$b9
000644506 7001_ $$aSchwarz, Alexander$$b10
000644506 7001_ $$0P:(DE-H253)PIP1010723$$aDippel, Ann-Christin$$b11
000644506 7001_ $$0P:(DE-H253)PIP1100821$$aIgoa Saldaña, Fernando$$b12
000644506 7001_ $$00000-0002-9768-647X$$aDetlefs, Blanka$$b13
000644506 7001_ $$0P:(DE-H253)PIP1031321$$aKoziej, Dorota$$b14$$eCorresponding author
000644506 773__ $$0PERI:(DE-600)1472210-0$$a10.1021/jacs.5c15843$$gVol. 147, no. 51, p. 47409 - 47420$$n51$$p47409 - 47420$$tJournal of the American Chemical Society$$v147$$x0002-7863$$y2025
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