论文标题
MAS DNP-NMR材料的最新发展
Recent developments in MAS DNP-NMR of materials
论文作者
论文摘要
固态NMR光谱是一种强大的技术,用于表征原子水平的结构和材料动力学。然而,这种技术的使用通常受到其缺乏灵敏度的限制,从而可以防止表面,缺陷或不敏感的同位素观察到。动态核极化(DNP)已被证明可以提高一到三个数量级,即在静态磁场上,NMR实验对魔法旋转(MAS)下的材料的灵敏度$ B_0 \ ge 5 $ T,允许获取高分辨率光谱。在过去的十年中,材料的DNP-NMR光谱领域经历了迅速发展,特别是由于商业DNP-NMR系统的可用性而刺激了。我们在这里提供了MAS DNP-NMR材料研究的深入概述,该研究高$ b_0 $ field。经过材料DNP的历史观点,我们描述了MAS下的DNP转移,自旋扩散通过极化的运输以及对DNP-NMR实验总体灵敏度的各种贡献。我们讨论了量身定制的偏振剂的设计和材料的样品制备。我们介绍DNP-NMR硬件以及关键实验参数的影响,例如微波功率,磁场,温度和MAS频率。我们概述了该技术检测到的同位素,以及与DNP结合的NMR方法。最后,我们展示了如何应用MAS DNP-NMR,以获得对有机,混合和无机材料结构的新见解,并在田野中应用,例如健康,能量,催化,光电子学等。
Solid-state NMR spectroscopy is a powerful technique for the characterization of the atomic-level structure and dynamics of materials. Nevertheless, the use of this technique is often limited by its lack of sensitivity, which can prevent the observation of surfaces, defects or insensitive isotopes. Dynamic Nuclear Polarization (DNP) has been shown to improve by one to three orders of magnitude the sensitivity of NMR experiments on materials under Magic-Angle Spinning (MAS), at static magnetic field $B_0 \ge 5$ T, conditions allowing for the acquisition of high-resolution spectra. The field of DNP-NMR spectroscopy of materials has undergone a rapid development in the last ten years, spurred notably by the availability of commercial DNP-NMR systems. We provide here an in-depth overview of MAS DNP-NMR studies of materials at high $B_0$ field. After a historical perspective of DNP of materials, we describe the DNP transfers under MAS, the transport of polarization by spin diffusion and the various contributions to the overall sensitivity of DNP-NMR experiments. We discuss the design of tailored polarizing agents and the sample preparation in the case of materials. We present the DNP-NMR hardware and the influence of key experimental parameters, such as microwave power, magnetic field, temperature and MAS frequency. We give an overview of the isotopes that have been detected by this technique, and the NMR methods that have been combined with DNP. Finally, we show how MAS DNP-NMR has been applied to gain new insights into the structure of organic, hybrid and inorganic materials with applications in fields, such as health, energy, catalysis,optoelectronics etc.