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Quantifying Ligand Exchange Reactions at CdSe Nanocrystal Surfaces
Chemistry of Materials ( IF 7.2 ) Pub Date : 2016-06-29 00:00:00 , DOI: 10.1021/acs.chemmater.6b01827 Robin R. Knauf 1 , J. Christian Lennox 1 , Jillian L. Dempsey 1
Chemistry of Materials ( IF 7.2 ) Pub Date : 2016-06-29 00:00:00 , DOI: 10.1021/acs.chemmater.6b01827 Robin R. Knauf 1 , J. Christian Lennox 1 , Jillian L. Dempsey 1
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The exchange reactions of X-type ligands at the surface of CdSe nanocrystals have been quantified via 1H NMR, absorbance, and emission spectroscopies. 1H NMR was used to quantify displacement reactions of oleate-capped CdSe nanocrystals with carboxylic-acid-, phosphonic-acid-, and thiol-terminated ligands that incorporate terminal alkene functionalities. The alkenyl protons of the native oleate ligand and the vinylic protons of the exchange ligand provide spectroscopic handles to quantify both free and surface-bound forms of these ligands. Undec-10-enoic acid was found to undergo an exchange equilibrium with oleate (Keq = 0.83), whereas phosphonic-acid- and thiol-terminated ligands irreversibly displace native oleate ligands. Absorption and emission experiments indicate that the carboxylic acid exchanges occur solely between surface-bound ligands, whereas exchange reactions with phosphonic acids and thiols alter the surface metal atoms of the nanocrystals, presumably through the displacement of Cd(oleate)2. These quantifications can be used to guide the selective functionalization of CdSe nanocrystals.
中文翻译：
量化CdSe纳米晶表面的配体交换反应
CdSe纳米晶体表面的X型配体的交换反应已通过1 H NMR，吸光度和发射光谱进行了定量。1 H NMR用于量化油酸酯封端的CdSe纳米晶体与羧酸，膦酸和巯基封端的配体的置换反应，这些配体具有末端烯烃官能团。天然油酸酯配体的烯基质子和交换配体的乙烯基质子提供了光谱学的方法以量化这些配体的游离形式和表面结合形式。发现十一碳烯酸与油酸酯发生交换平衡（K eq= 0.83），而膦酸和巯基封端的配体不可逆地取代了天然油酸酯配体。吸收和发射实验表明，羧酸交换仅发生在表面结合的配体之间，而与膦酸和硫醇的交换反应则可能是通过Cd（油酸酯）2的置换而改变了纳米晶体的表面金属原子。这些量化可用于指导CdSe纳米晶体的选择性功能化。
更新日期：2016-06-29
中文翻译：
量化CdSe纳米晶表面的配体交换反应
CdSe纳米晶体表面的X型配体的交换反应已通过1 H NMR，吸光度和发射光谱进行了定量。1 H NMR用于量化油酸酯封端的CdSe纳米晶体与羧酸，膦酸和巯基封端的配体的置换反应，这些配体具有末端烯烃官能团。天然油酸酯配体的烯基质子和交换配体的乙烯基质子提供了光谱学的方法以量化这些配体的游离形式和表面结合形式。发现十一碳烯酸与油酸酯发生交换平衡（K eq= 0.83），而膦酸和巯基封端的配体不可逆地取代了天然油酸酯配体。吸收和发射实验表明，羧酸交换仅发生在表面结合的配体之间，而与膦酸和硫醇的交换反应则可能是通过Cd（油酸酯）2的置换而改变了纳米晶体的表面金属原子。这些量化可用于指导CdSe纳米晶体的选择性功能化。
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