The UK High-Field Solid-State NMR National Research Facility: EPSRC Core Equipment Award 2022

英国高场固态核磁共振国家研究设施：2022 年 EPSRC 核心设备奖

• 批准号: EP/X03481X/1
• 负责人: Steven Brown
• 金额: $ 61.49万
• 依托单位: University of Warwick
• 依托单位国家: 英国
• 项目类别: Research Grant
• 财政年份: 2023
• 资助国家: 英国
• 起止时间: 2023 至 无数据
• 项目状态: 未结题
• 来源: https://gtr.ukri.org/projects?ref=EP%2FX03481X%2F1
• 关键词: UK; Field; Solid; State; NMR

Solid-state nuclear magnetic resonance (NMR) spectroscopy is arguably the most powerful technology for providing atomic-level structure and dynamics understanding of molecules and materials. The physical and life sciences communities exploit this analytical science technique extensively to address challenging issues in a wide range of systems relevant to, for example, pharmaceuticals, battery materials, catalysis and protein complexes. Importantly, the advances enabled by solid-state NMR as an analytical technique are continually increasing in line with technological progresses in the development of new NMR hardware. The importance of solid-state NMR is reflected in investment in the UK High-Field Solid-State NMR National Research Facility (NRF). Breakthroughs in NMR hardware development have often been in the design of magic-angle spinning (MAS) probes. MAS improve both the sensitivity and resolution of NMR spectra by physical rotation of the sample at very high frequencies (up to about 150,000 revolutions per second) to remove the effects of interactions that broaden and complicate solid-state NMR spectra. At the same time, it is often desirable to perform NMR measurements at a range of different temperatures to give insight into temperature-driven structural changes, or to characterise and quantify motional processes in materials. Standard MAS probes can typically achieve sample temperatures in the range -80 to +100 C, but it is often necessary to perform measurements outside of this range depending on the nature of the motional/structural phenomena and interactions present. Recent developments in probe design have resulted in the availability of laser-heated probes capable of heating to ~1000 K and cryogen-cooled probes capable of cooling to ~100 K. This represents a significant widening of the accessible temperature range and provides an exciting opportunity to study structure and dynamics in unprecedented detail. Of the two high-field spectrometers within the NRF, the wide-bore design of the 850 MHz spectrometer allows for challenging experiments with non-standard probe designs. As part of the 2020-4 NRF investment, funding to purchase a laser-heated MAS probe for the 850 MHz spectrometer was secured and the probe was installed in early 2022 with already successful outputs. Here, we propose to further extend the capability and impact of this world-leading facility with the purchase of a state-of-the-art cryogenically-cooled low-temperature (LT)MAS probe capable of performing measurements at cryogenic temperatures down to 100 K. The combination of this probe with the existing laser-heated probe will maximise the available temperature range for MAS experiments, giving researchers increased access to dynamic and structural phenomena, while at the same time maximising resolution and sensitivity due to the high magnetic field. Due to the Botzmann distribution, the LTMAS setup itself also provides an intrinsic factor of three sensitivity enhancement (corresponding to a factor of 9 reduction in experimental time) which will enable new experiments to be performed that were previously unfeasible due to poor sensitivity. These advantages will potentially impact all systems studied at the NRF, but will be particularly beneficial for the study of low-sensitivity quadrupolar nuclei, which are of great importance in materials science, but suffer from additional broadening that complicate their observation at low magnetic fields.The highly experienced Facility Management Team will ensure that the LTMAS probe is exploited to its maximum capabilities. The NRF has active program of engaging actions with the UK NMR community and beyond, most notably via the Connect NMR UK network and the Facility's existing activities in outreach, to promote and raise awareness of the new hardware capabilities and to grow and diversify its user base.

固态核磁共振（NMR）光谱可以说是提供原子级结构和对分子和材料的动态理解的最强大技术。物理和生命科学社区广泛利用了这种分析科学技术，以解决与药品，电池材料，催化和蛋白质复合物相关的广泛系统中的挑战性问题。重要的是，固态NMR作为一种分析技术的进步不断增加，随着新NMR硬件的开发的技术进步。固态NMR的重要性反映在英国高级固态NMR国家研究机构（NRF）的投资中。 NMR硬件开发中的突破通常是在魔术角旋转（MAS）探针的设计中。 MAS通过在非常高的频率（每秒大约150,000转）的物理旋转（每秒大约150,000转）的物理旋转来提高NMR光谱的灵敏度和分辨率，以消除扩大和复杂化固态NMR光谱的相互作用的影响。同时，通常希望在各种温度下进行NMR测量，以深入了解温度驱动的结构变化，或表征和量化材料中的运动过程。标准MAS探针通常可以在-80至+100 C范围内实现样品温度，但是通常有必要根据存在的运动/结构现象和相互作用的性质进行测量。探针设计的最新发展导致了能够加热至约1000 K的激光加热探针以及能够冷却至〜100 k的低温冷却探针的可用性。这代表了可访问的温度范围的显着扩大，并为研究结构和动态提供了令人兴奋的机会，以无前前细节研究。在NRF内的两个高场光谱仪中，850 MHz光谱仪的宽孔设计允许通过非标准探针设计进行具有挑战性的实验。作为2020-4 NRF投资的一部分，确保了为850 MHz光谱仪购买激光加热的MAS探测器的资金，并在2022年初安装了探测器，并以已成功的输出为止。在这里，我们建议通过购买最先进的低温冷却低温（LT）MAS探测器，能够在低温温度下进行测量至100 K的高温冷却低温（LT）MAS探测，以进一步扩展这种世界领先的设施的能力和影响。同一时间由于高磁场而导致的分辨率和灵敏度最大化。由于Botzmann分布，LTMAS设置本身还提供了三种灵敏度增强的内在因素（对应于实验时间减少9倍），这将使由于敏感性较差而以前无法进行新实验。这些优势可能会影响NRF研究的所有系统，但对于研究低敏感性四极核的研究尤其有益，这在材料科学中非常重要，但是遭受了额外的扩展，使其在低磁场上的观察变得复杂。 NRF具有与英国NMR社区及以后的行动的积极计划，最著名的是通过连接NMR UK Network以及该设施在外展中的现有活动，以促进和提高人们对新硬件功能的认识，并增长和多样化其用户群。