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000622040 245__ $$aUtilizing High X-ray Energy Photon-In Photon-Out Spectroscopies and X-ray Scattering to Experimentally Assess the Emergence of Electronic and Atomic Structure of ZnS Nanorods
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000622040 520__ $$aThe key to controlling the fabrication process of transition metal sulfide nanocrystals is to understand the reaction mechanism, especially the coordination of ligands and solvents during their synthesis. We utilize in situ high-energy resolution fluorescence detected X-ray absorption spectroscopy (HERFD-XAS) as well as in situ valence-to-core X-ray emission spectroscopy (vtc-XES) combined with density functional theory (DFT) calculations to identify the formation of a tetrahedral [Zn(OA)$_4$]$^{2+}$ and an octahedral [Zn(OA)$_6$]$^{2+}$ complex, and the ligand exchange to a tetrahedral [Zn(SOA)$_4$]$^{2+}$ complex (OA = oleylamine, OAS = oleylthioamide), during the synthesis of ZnS nanorods in oleylamine. We observe in situ the transition of the electronic structure of [Zn(SOA)$_4$]$^{2+}$ with a HOMO/LUMO gap of 5.0 eV toward an electronic band gap of 4.3 and 3.8 eV for 1.9 nm large ZnS wurtzite nanospheres and 2 × 7 nm sphalerite nanorods, respectively. Thus, we demonstrate how in situ multimodal X-ray spectroscopy and scattering studies can not only resolve structure, size, and shape during the growth and synthesis of NPs in organic solvents and at high temperature but also give direct information about their electronic structure, which is not readily accessible through other techniques.  
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000622040 7001_ $$0P:(DE-H253)PIP1098796$$aGröne, Tjark L. R.$$b1
000622040 7001_ $$0P:(DE-H253)PIP1085597$$aZito, Cecilia de Almeida$$b2
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000622040 7001_ $$0P:(DE-HGF)0$$aGumus Akcaalan, Melike$$b4
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000622040 7001_ $$0P:(DE-H253)PIP1099470$$aSteenbock, Torben$$b7
000622040 7001_ $$0P:(DE-HGF)0$$aHussak, Sarah-Alexandra$$b8
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000622040 7001_ $$0P:(DE-H253)PIP1010723$$aDippel, Ann-Christin$$b10$$udesy
000622040 7001_ $$0P:(DE-H253)PIP1018539$$aSun, Xiao$$b11$$udesy
000622040 7001_ $$0P:(DE-HGF)0$$aKöppen, Andrea$$b12
000622040 7001_ $$0P:(DE-HGF)0$$aSaveleva, Viktoriia A.$$b13
000622040 7001_ $$0P:(DE-HGF)0$$aKumar, Surender$$b14
000622040 7001_ $$0P:(DE-H253)PIP1098109$$aBester, Gabriel$$b15
000622040 7001_ $$00000-0001-6532-8144$$aGlatzel, Pieter$$b16
000622040 7001_ $$0P:(DE-H253)PIP1031321$$aKoziej, Dorota$$b17$$eCorresponding author
000622040 77318 $$2Crossref$$3journal-article$$a10.1021/jacs.4c10257$$bAmerican Chemical Society (ACS)$$d2024-11-25$$n49$$p33475-33484$$tJournal of the American Chemical Society$$v146$$x0002-7863$$y2024
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