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000636202 1001_ $$0P:(DE-H253)PIP1083268$$aKlemeyer, Lars$$b0$$udesy
000636202 245__ $$aSpatially Resolved In Situ X-ray Absorption Spectroscopy Studies of ZnS Nanoparticle Synthesis at the Water–Toluene Interface
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000636202 520__ $$aTwo-phase synthesis is a well-established approach for achieving precise control of the nanoparticle properties. However, studying and understanding chemical transformations in such a spatially heterogeneous system is challenging. In this work, we introduce a two-phase synthesis route for ZnS nanoparticles (ZnS NPs) at the water–toluene interface. By employing spatially resolved in situ high-energy resolution fluorescence-detected X-ray absorption spectroscopy (HERFD-XAS) combined with density functional theory (DFT) calculations, we track the diffusion of Zn$^{2+}$ species at the interface, identify key reaction intermediates, and monitor the nucleation and growth of ZnS NPs within the toluene phase. We propose the formation of a [Zn(H$_2$O)$_6$]$^{2+}$ complex upon dissolving Zn(Ac)$_2$ in water and the diffusion of Zn$^{2+}$ ions from water to toluene driven by the formation of an octahedral [Zn(OA)$_6$]$^{2+}$ complex (OA = oleylamine). Furthermore, by complementing HERFD-XAS with total X-ray scattering analysis, we show the formation of an intermediate tetrahedral [Zn(SR)4]$^{2+}$ complex at 60 °C and its successive transformation to noncrystalline ZnS nuclei at 80 °C and crystalline ZnS NPs starting at 100 °C. Thus, we demonstrate how in situ X-ray spectroscopy can elucidate the coordination and diffusion of Zn$^{2+}$ ions, and, in combination with X-ray scattering studies, identify the emergence of atomic and electronic structures during the two-phase synthesis of ZnS nanoparticles.  
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000636202 7001_ $$0P:(DE-H253)PIP1092080$$aCaddeo, Francesco$$b1
000636202 7001_ $$0P:(DE-H253)PIP1098796$$aGröne, Tjark L. R.$$b2
000636202 7001_ $$0P:(DE-H253)PIP1083208$$aHarouna-Mayer, Sani Y.$$b3
000636202 7001_ $$0P:(DE-H253)PIP1090769$$aJessen, Brian$$b4
000636202 7001_ $$0P:(DE-H253)PIP1085597$$aZito, Cecilia A.$$b5
000636202 7001_ $$0P:(DE-H253)PIP1085745$$aKopula Kesavan, Jagadesh$$b6
000636202 7001_ $$0P:(DE-H253)PIP1010723$$aDippel, Ann-Christin$$b7$$udesy
000636202 7001_ $$0P:(DE-H253)PIP1100821$$aIgoa Saldana, Fernando$$b8$$udesy
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000636202 7001_ $$00000-0001-6532-8144$$aGlatzel, Pieter$$b10
000636202 7001_ $$0P:(DE-H253)PIP1031321$$aKoziej, Dorota$$b11$$eCorresponding author
000636202 773__ $$0PERI:(DE-600)2383064-5$$a10.1021/acsnano.5c02875$$gVol. 19, no. 28, p. 25710 - 25719$$n28$$p25710 - 25719$$tACS nano$$v19$$x1936-0851$$y2025
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