Solid-State Nuclear Magnetic Resonance (NMR) Spectroscopy of Unreceptive Nuclei from Across the Periodic Table

在化学系化学测量和成像计划的支持下，以及材料研究部固体和材料化学计划的部分共同资助下，佛罗里达州立大学的罗伯特·舒尔科教授和他的团队正在努力扩大固态核磁共振(SS核磁共振)的适用范围，固态核磁共振是分析各种化合物、生物样品和先进材料的重要工具。许多用SS核磁共振可能观察到的原子据说是不可接受的，这意味着数据采集可能需要几天、几周甚至几个月的时间才能完成。Schurko小组正在开发的新方法极大地加速了核磁共振实验，从而扩展了我们表征对社会重要的材料的分子结构的能力。这种认识的增加反过来可以导致药物、催化剂、纳米粒子、含能材料和其他材料的改进。从事这项研究的本科生和研究生接受最先进的测量科学的跨学科培训。舒尔科博士还参与了国家强磁场实验室(MagLab)的STEM推广活动，在那里他是核磁共振和磁共振成像用户计划的主任。这些努力旨在让公众了解核磁共振，包括面向高中生的MagLab实习计划，面向教师的K-12研究经验，以及磁力学院计划。这些项目吸引了来自不同社会经济背景的不同群体。Schurko小组专注于开发和应用新方法，以获取来自元素周期表中元素的不可接受核的具有超宽线模式的高质量SS核磁共振谱，旨在最大化统一信号，减少数据采集时间，并提高最终用户的执行简易性。目前正在制定协议，通过实验和模拟相结合的方式，仔细监测核自旋行为。新的脉冲序列和实验方案在直接激发/直接探测、宽带交叉极化和间接探测方法等一般领域中针对自旋1/2核、整数自旋核和半整数自旋核。这项研究需要仔细考虑脉冲持续时间和定时，并使用专门设计的扫频脉冲。针对最难接受的核的项目利用超高磁场-包括35.2特斯拉系列连接的混合磁铁。所有新方法都提供给来自许多学科的研究人员(包括专家和非专家)，他们可以使用它们来表征固体材料的结构。该奖项反映了NSF的法定使命，并通过使用基金会的智力优势和更广泛的影响审查标准进行评估，被认为值得支持。

With support from the Chemical Measurement and Imaging Program in the Division of Chemistry, and partial co-funding from the Solid State and Materials Chemistry Program in the Division of Materials Research, Professor Robert Schurko and his group at Florida State University are working to expand the range of applicability of solid-state nuclear magnetic resonance (SSNMR), an important tool for the analysis of a wide range of chemical compounds, biological samples, and advanced materials. Many kinds of atoms potentially observable with SSNMR are said to be unreceptive, meaning that data acquisition can take days, weeks, or even months to complete. The new methods being developed by the Schurko group accelerate the NMR experiments greatly, thereby expanding our ability to characterize the molecular level structures of materials important to society. This increase in understanding can, in turn, lead to improved pharmaceuticals, catalysts, nanoparticles, energetic materials, and other materials. Undergraduate and graduate students engaged in this research receive interdisciplinary training in state-of-the-art measurement science. Dr. Schurko is also involved in STEM outreach activities at the National High Magnetic Field Laboratory (MagLab), where he is the Director of the NMR and Magnetic Resonance Imaging User Program. These efforts seek to inform the general public about NMR, and include MagLab internship programs for high school students, K-12 Research Experiences for Teachers, and the Magnet Academy Program. These programs engage diverse groups of people from different socioeconomic backgrounds. The Schurko group focuses on the development and application of new methods for the acquisition of high-quality SSNMR spectra with ultra-wideline patterns originating from unreceptive nuclei from elements across the periodic table, aiming at maximizing uniform signal, reducing data acquisition times, and improving ease of execution for end users. Protocols are being developed to carefully monitor nuclear spin behavior via a combination of experiments and simulations. New pulse sequences and experimental protocols are targeting spin-1/2, integer-spin, and half-integer spin nuclei in the general areas of direct excitation/direct detection, broadband cross polarization, and indirect detection methods. This research requires careful consideration of pulse durations and timings, and the use of specially designed frequency-swept pulses. Projects targeting the most unreceptive nuclei exploit ultra-high magnetic fields – including the 35.2 Tesla series-connected hybrid magnet. All new methods are made available to researchers from many disciplines (both experts and non-experts), who can use them for structural characterization of solid materials.This award reflects NSF's statutory mission and has been deemed worthy of support through evaluation using the Foundation's intellectual merit and broader impacts review criteria.