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 B₀ ≥ 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 B₀ 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.

固态NMR光谱学是一种用于表征原子级结构和材料动力学的强大技术。但是，由于缺乏灵敏性，该技术的使用常常受到限制，因为它可能无法观察到表面，缺陷或不敏感的同位素。研究表明，动态核极化（DNP）可以在静磁场B ₀下在魔角旋转（MAS）下对材料进行NMR实验的灵敏度提高1-3个数量级。 ≥5 T，允许采集高分辨率光谱的条件。在过去的十年中，材料的DNP-NMR光谱学领域得到了飞速发展，尤其是受到商业化DNP-NMR系统的推动。我们在此提供有关高B ₀下材料的MAS DNP-NMR研究的深入概述。领域。从材料的DNP的历史角度出发，我们描述了MAS下的DNP转移，通过自旋扩散的极化传输以及对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以及在材料情况下的样品制备。我们介绍了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。我们概述了通过这种技术检测到的同位素，以及与DNP结合的NMR方法。最后，我们展示了如何将MAS DNP-NMR应用于健康，能源，催化，光电等领域的有机，杂化和无机材料结构的新见解。