Triple resonance solid-state NMR for multi-nuclear studies

用于多核研究的三重共振固态核磁共振

• 批准号: 345369-2007
• 负责人: Goward, Gillian
• 金额: $ 10.93万
• 依托单位: McMaster University
• 依托单位国家: 加拿大
• 项目类别: Research Tools and Instruments - Category 1 (<$150,000)
• 财政年份: 2006
• 资助国家: 加拿大
• 起止时间: 2006-01-01 至 2007-12-31
• 项目状态: 已结题
• 来源: https://www.nserc-crsng.gc.ca/ase-oro/Details-Detailles_eng.asp?id=325961
• 关键词: Triple; resonance; solid; state; NMR

The suite of equipment requested here will enable triple resonance nuclear magnetic resonance (NMR) spectroscopy on our solid-state AV 500 NMR spectrometer.  The critical components include the triple resonance 4mm magic angle spinning probe (1H/19F, X, Y) and the 500W amplifier for a third channel, as well as the accompanying hardware for incorporating a third channel into the existing spectrometer console.  This new equipment will meet the needs of several research projects within our group, and significantly expand the capacity of this spectrometer.      Rechargeable lithium polymer batteries find many uses in portable electronics, and are poised to lead major breakthroughs in the area of zero emission vehicles.  The success of new materials is governed by their ability to reversibly transport lithium ions.  A class of cathode materials which have received much attention lately are the transition metal phosphates, which have open framework structures that facilitate ion transport.  The measurement of residual dipolar couplings is powerful method for characterizing local dynamics, well-known in the protein NMR community, but pioneered in our group in its application to solid-state ionic conductors. The new suite of equipment will allow us to investigate lithium ion dynamics using a new spectroscopic handle, namely the 6Li-31P dipolar coupling.      Polymer-electrolyte membranes for fuel cells, which can provide environmentally friendly energy, rely on membranes able to conduct protons. Many of the competitive polymer candidates are perfluorinated materials.  The probe requested here will facilitate excellent 19F NMR, at MAS frequencies of 24kHz, sufficient to eliminate sidebands from the spectral region of interest.  The new probe will allow us to characterize backbone dynamics in Nafion and its numerous analogues, by measuring both 19F directly, and 19F-13C cross polarization enhanced spectra.  New collaborations with synthetic groups who are designing novel fluorinated proton-conducting polymers will be enabled.

这里要求的一套设备将在我们的固态AV 500核磁共振光谱仪上实现三重共振核磁共振(核磁共振)波谱。关键部件包括三重共振4 mm魔角旋转探头(1H/19F，X，Y)和用于第三个通道的500W放大器，以及用于将第三个通道整合到现有光谱仪控制台的配套硬件。我们相信，这台新设备将满足我们集团内几个研究项目的需求，并显著扩大该光谱仪的容量。目前，可充电锂聚合物电池在便携式电子产品中有许多用途，并有望在零排放汽车领域取得重大突破。新材料的成功取决于它们可逆传输锂离子的能力。最近备受关注的一类正极材料是过渡金属磷酸盐，它具有开放的框架结构，有助于离子传输。剩余偶极耦合的测量是表征局部动力学的有力方法，在蛋白质核磁共振界是众所周知的，但在我们小组将其应用于固态离子导体方面是首创。这套新的设备将允许我们使用一种新的光谱手柄，即6Li-31P偶极耦合来研究锂离子的动力学。目前，用于燃料电池的聚合物-电解质膜可以提供环境友好的能源，依赖于能够传导质子的膜。许多竞争的候选聚合物都是全氟材料。这里要求的探测器将有助于在24 kHz的MAS频率下实现出色的19F核磁共振，足以从感兴趣的光谱区域消除边带。新探测器将允许我们通过直接测量19F和19F-13C交叉极化增强光谱来表征Nafion及其众多类似物的主干动力学。*将能够与设计新型氟化质子导电聚合物的合成小组进行新的合作。