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Sensitivity-Enhanced 207Pb Solid-State NMR Spectroscopy for the Rapid, Non-Destructive Characterization of Organolead Halide Perovskites
Chemistry of Materials ( IF 7.2 ) Pub Date : 2018-09-18 00:00:00 , DOI: 10.1021/acs.chemmater.8b01899 Michael P. Hanrahan 1, 2 , Long Men 1, 2 , Bryan A. Rosales 1 , Javier Vela 1, 2 , Aaron J. Rossini 1, 2
Chemistry of Materials ( IF 7.2 ) Pub Date : 2018-09-18 00:00:00 , DOI: 10.1021/acs.chemmater.8b01899 Michael P. Hanrahan 1, 2 , Long Men 1, 2 , Bryan A. Rosales 1 , Javier Vela 1, 2 , Aaron J. Rossini 1, 2
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Organolead halide and mixed halide perovskites (CH3NH3PbX3, CH3NH3PbX3–nYn, X and Y = Cl–, Br–, or I–) are promising materials for photovoltaics and optoelectronic devices. 207Pb solid-state NMR spectroscopy has previously been applied to characterize phase segregation and halide ion speciation in mixed halide perovskites. However, NMR spectroscopy is an insensitive technique that often requires large sample volumes and long signal averaging periods. This is especially true for mixed halide perovskites, which give rise to extremely broad 207Pb solid-state NMR spectra. Here, we quantitatively compare the sensitivity of the various solid-state NMR techniques on pure and mixed halide organolead perovskites and demonstrate that both fast MAS and DNP can provide substantial gains in NMR sensitivity for these materials. With fast MAS and proton detection, high signal-to-noise ratio two-dimensional (2D) 207Pb–1H heteronuclear correlation (HETCOR) NMR spectra can be acquired in less than half an hour from only ca. 4 μL of perovskite material. Modest relayed DNP enhancements on the order of 1 to 20 were obtained for perovskites. The cryogenic temperatures (110 K) used for DNP experiments also provide a significant boost in sensitivity. Consequently, it was possible to obtain the 207Pb solid-state NMR spectrum of a 300 nm thick model thin film of CH3NH3PbI3 in 34 h by performing solid-state NMR experiments with a sample temperature of 110 K. This result demonstrates the possibility of using NMR spectroscopy for characterization of perovskite thin films.
中文翻译：
灵敏度增强的207 Pb固态NMR光谱用于有机油脂卤化物钙钛矿的快速，非破坏性表征
有机油卤化物和混合卤化物钙钛矿（CH 3 NH 3 PbX 3，CH 3 NH 3 PbX 3– n Y n，X和Y = Cl –，Br –或I –）是用于光伏和光电器件的有前途的材料。先前已将207 Pb固态NMR光谱用于表征混合卤化物钙钛矿中的相偏析和卤离子形态。但是，NMR光谱学是一种不灵敏的技术，通常需要大量的样本量和较长的信号平均周期。对于混合卤化物钙钛矿来说尤其如此，因为它引起了广泛的应用。207 Pb固态NMR光谱。在这里，我们定量比较了各种固态NMR技术对纯卤化物和混合卤化物有机铅钙钛矿的敏感性，并证明快速MAS和DNP均可为这些材料提供NMR灵敏度的实质性提高。通过快速的MAS和质子检测，仅在大约半小时内即可获得高信噪比的二维（2D）207 Pb– 1 H异核相关（HETCOR）NMR光谱。4μL钙钛矿材料。钙钛矿获得了适度的DNP增强，数量级为1至20。用于DNP实验的低温（110 K）也大大提高了灵敏度。因此，有可能获得207通过在110 K的样品温度下进行固态NMR实验，在34小时内对CH 3 NH 3 PbI 3的300 nm厚模型薄膜的Pb固态NMR光谱。该结果表明使用NMR光谱进行表征的可能性钙钛矿薄膜。
更新日期：2018-09-18
中文翻译：
灵敏度增强的207 Pb固态NMR光谱用于有机油脂卤化物钙钛矿的快速，非破坏性表征
有机油卤化物和混合卤化物钙钛矿（CH 3 NH 3 PbX 3，CH 3 NH 3 PbX 3– n Y n，X和Y = Cl –，Br –或I –）是用于光伏和光电器件的有前途的材料。先前已将207 Pb固态NMR光谱用于表征混合卤化物钙钛矿中的相偏析和卤离子形态。但是，NMR光谱学是一种不灵敏的技术，通常需要大量的样本量和较长的信号平均周期。对于混合卤化物钙钛矿来说尤其如此，因为它引起了广泛的应用。207 Pb固态NMR光谱。在这里，我们定量比较了各种固态NMR技术对纯卤化物和混合卤化物有机铅钙钛矿的敏感性，并证明快速MAS和DNP均可为这些材料提供NMR灵敏度的实质性提高。通过快速的MAS和质子检测，仅在大约半小时内即可获得高信噪比的二维（2D）207 Pb– 1 H异核相关（HETCOR）NMR光谱。4μL钙钛矿材料。钙钛矿获得了适度的DNP增强，数量级为1至20。用于DNP实验的低温（110 K）也大大提高了灵敏度。因此，有可能获得207通过在110 K的样品温度下进行固态NMR实验，在34小时内对CH 3 NH 3 PbI 3的300 nm厚模型薄膜的Pb固态NMR光谱。该结果表明使用NMR光谱进行表征的可能性钙钛矿薄膜。
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