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\n  \n 2024\n \n \n (2)\n \n \n
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\n \n\n \n \n \n \n \n \n On the Fate of Lithium Ions in Sol–Gel Derived Zinc Oxide Nanocrystals.\n \n \n \n \n\n\n \n Olejnik‐Fehér, N.; Jędrzejewska, M.; Wolska‐Pietkiewicz, M.; Lee, D.; Paëpe, G. D.; and Lewiński, J.\n\n\n \n\n\n\n Small,2309984. March 2024.\n \n\n\n\n
\n\n\n\n \n \n \"OnPaper\n  \n \n\n \n \n doi\n  \n \n\n \n link\n  \n \n\n bibtex\n \n\n \n  \n \n abstract \n \n\n \n\n \n \n \n \n \n \n \n\n  \n \n \n \n \n \n \n \n \n \n \n \n \n\n\n\n
\n 
@article{olejnikfeher_fate_2024,\n\ttitle = {On the {Fate} of {Lithium} {Ions} in {Sol}–{Gel} {Derived} {Zinc} {Oxide} {Nanocrystals}},\n\tissn = {1613-6810, 1613-6829},\n\turl = {https://onlinelibrary.wiley.com/doi/10.1002/smll.202309984},\n\tdoi = {10.1002/smll.202309984},\n\tabstract = {Abstract\n            \n              Among diverse chemical synthetic approaches to zinc oxide nanocrystals (ZnO NCs), ubiquitous inorganic sol–gel methodology proved crucial for advancements in ZnO‐based nanoscience. Strikingly, unlike the exquisite level of control over morphology and size dispersity achieved in ZnO NC syntheses, the purity of the crystalline phase, as well as the understanding of the surface structure and the character of the inorganic–organic interface, have been limited to vague descriptors until very recently. Herein, ZnO NCs applying the standard sol–gel synthetic protocol are synthesized with zinc acetate and lithium hydroxide and tracked the integration of lithium (Li) cations into the interior and exterior of nanoparticles by combining various techniques, including advanced solid‐state NMR methods. In contrast to common views, it is demonstrated that Li\n              +\n              ions remain kinetically trapped in the inorganic core, enter into a shallow subsurface layer, and generate “swelling” of the surface and interface regions. Thus, this work enabled both the determination of the NCs’ structural imperfections and an in‐depth understanding of the unappreciated role of the Li\n              +\n              ions in impacting the doping and the passivation of sol–gel‐derived ZnO nanomaterials.},\n\tlanguage = {en},\n\turldate = {2024-04-08},\n\tjournal = {Small},\n\tauthor = {Olejnik‐Fehér, Natalia and Jędrzejewska, Maria and Wolska‐Pietkiewicz, Małgorzata and Lee, Daniel and Paëpe, Gaël De and Lewiński, Janusz},\n\tmonth = mar,\n\tyear = {2024},\n\tkeywords = {lithium, nanocrystals, solid-state NMR, sol–gel, zinc oxide},\n\tpages = {2309984},\n}\n\n
\n
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\n Abstract Among diverse chemical synthetic approaches to zinc oxide nanocrystals (ZnO NCs), ubiquitous inorganic sol–gel methodology proved crucial for advancements in ZnO‐based nanoscience. Strikingly, unlike the exquisite level of control over morphology and size dispersity achieved in ZnO NC syntheses, the purity of the crystalline phase, as well as the understanding of the surface structure and the character of the inorganic–organic interface, have been limited to vague descriptors until very recently. Herein, ZnO NCs applying the standard sol–gel synthetic protocol are synthesized with zinc acetate and lithium hydroxide and tracked the integration of lithium (Li) cations into the interior and exterior of nanoparticles by combining various techniques, including advanced solid‐state NMR methods. In contrast to common views, it is demonstrated that Li + ions remain kinetically trapped in the inorganic core, enter into a shallow subsurface layer, and generate “swelling” of the surface and interface regions. Thus, this work enabled both the determination of the NCs’ structural imperfections and an in‐depth understanding of the unappreciated role of the Li + ions in impacting the doping and the passivation of sol–gel‐derived ZnO nanomaterials.\n
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\n \n\n \n \n \n \n \n \n AsymPol-TEKs as efficient polarizing agents for MAS-DNP in glass matrices of non-aqueous solvents.\n \n \n \n \n\n\n \n Harrabi, R.; Halbritter, T.; Alarab, S.; Chatterjee, S.; Wolska-Pietkiewicz, M.; Damodaran, K. K.; Van Tol, J.; Lee, D.; Paul, S.; Hediger, S.; Sigurdsson, S. T.; Mentink-Vigier, F.; and De Paëpe, G.\n\n\n \n\n\n\n Physical Chemistry Chemical Physics, 26(6): 5669–5682. 2024.\n \n\n\n\n
\n\n\n\n \n \n \"AsymPol-TEKsPaper\n  \n \n\n \n \n doi\n  \n \n\n \n link\n  \n \n\n bibtex\n \n\n \n  \n \n abstract \n \n\n \n\n \n \n \n \n \n \n \n\n  \n \n \n\n\n\n
\n 
@article{harrabi_asympol-teks_2024,\n\ttitle = {{AsymPol}-{TEKs} as efficient polarizing agents for {MAS}-{DNP} in glass matrices of non-aqueous solvents},\n\tvolume = {26},\n\tissn = {1463-9076, 1463-9084},\n\turl = {http://xlink.rsc.org/?DOI=D3CP04271E},\n\tdoi = {10.1039/D3CP04271E},\n\tabstract = {Two polarizing agents from the AsymPol family, AsymPol-TEK and cAsymPol-TEK (methyl-free version) are introduced for MAS-DNP applications in non-aqueous solvents.\n          , \n            \n              Two polarizing agents from the AsymPol family, AsymPol-TEK and cAsymPol-TEK (methyl-free version) are introduced for MAS-DNP applications in non-aqueous solvents. The performance of these new biradicals is rationalized in detail using a combination of electron paramagnetic resonance spectroscopy, density functional theory, molecular dynamics and quantitative MAS-DNP spin dynamics simulations. By slightly modifying the experimental protocol to keep the sample temperature low at insertion, we are able to obtain reproducable DNP-NMR data with 1,1,2,2-tetrachloroethane (TCE) at 100 K, which facilitates optimization and comparison of different polarizing agents. At intermediate magnetic fields, AsymPol-TEK and cAsymPol-TEK provide 1.5 to 3-fold improvement in sensitivity compared to TEKPol, one of the most widely used polarizing agents for organic solvents, with significantly shorter DNP build-up times of ∼1 s and ∼2 s at 9.4 and 14.1 T respectively. In the course of the work, we also isolated and characterized two diastereoisomers that can form during the synthesis of AsymPol-TEK; their difference in performance is described and discussed. Finally, the advantages of the AsymPol-TEKs are demonstrated by recording 2D\n              13\n              C–\n              13\n              C correlation experiments at natural\n              13\n              C-abundance of proton-dense microcrystals and by polarizing the surface of ZnO nanocrystals (NCs) coated with diphenyl phosphate ligands. For those experiments, cAsymPol-TEK yielded a three-fold increase in sensitivity compared to TEKPol, corresponding to a nine-fold time saving.},\n\tlanguage = {en},\n\tnumber = {6},\n\turldate = {2024-04-08},\n\tjournal = {Physical Chemistry Chemical Physics},\n\tauthor = {Harrabi, Rania and Halbritter, Thomas and Alarab, Shadi and Chatterjee, Satyaki and Wolska-Pietkiewicz, Malgorzata and Damodaran, Krishna K. and Van Tol, Johan and Lee, Daniel and Paul, Subhradip and Hediger, Sabine and Sigurdsson, Snorri Th. and Mentink-Vigier, Frederic and De Paëpe, Gaël},\n\tyear = {2024},\n\tpages = {5669--5682},\n}\n\n
\n
\n\n\n
\n Two polarizing agents from the AsymPol family, AsymPol-TEK and cAsymPol-TEK (methyl-free version) are introduced for MAS-DNP applications in non-aqueous solvents. , Two polarizing agents from the AsymPol family, AsymPol-TEK and cAsymPol-TEK (methyl-free version) are introduced for MAS-DNP applications in non-aqueous solvents. The performance of these new biradicals is rationalized in detail using a combination of electron paramagnetic resonance spectroscopy, density functional theory, molecular dynamics and quantitative MAS-DNP spin dynamics simulations. By slightly modifying the experimental protocol to keep the sample temperature low at insertion, we are able to obtain reproducable DNP-NMR data with 1,1,2,2-tetrachloroethane (TCE) at 100 K, which facilitates optimization and comparison of different polarizing agents. At intermediate magnetic fields, AsymPol-TEK and cAsymPol-TEK provide 1.5 to 3-fold improvement in sensitivity compared to TEKPol, one of the most widely used polarizing agents for organic solvents, with significantly shorter DNP build-up times of ∼1 s and ∼2 s at 9.4 and 14.1 T respectively. In the course of the work, we also isolated and characterized two diastereoisomers that can form during the synthesis of AsymPol-TEK; their difference in performance is described and discussed. Finally, the advantages of the AsymPol-TEKs are demonstrated by recording 2D 13 C– 13 C correlation experiments at natural 13 C-abundance of proton-dense microcrystals and by polarizing the surface of ZnO nanocrystals (NCs) coated with diphenyl phosphate ligands. For those experiments, cAsymPol-TEK yielded a three-fold increase in sensitivity compared to TEKPol, corresponding to a nine-fold time saving.\n
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