Very Low Field 2.35 T Solid State NMR Console and Fast MAS NMR Probe for the Study of Paramagnetic Materials Systems

用于研究顺磁性材料系统的极低场 2.35 T 固态 NMR 控制台和快速 MAS NMR 探头

• 批准号: EP/K024418/1
• 负责人: John Hanna
• 金额: $ 8.28万
• 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: 2013
• 资助国家: 英国
• 起止时间: 2013 至 无数据
• 项目状态: 已结题
• 来源: https://gtr.ukri.org/projects?ref=EP%2FK024418%2F1
• 关键词: Very; Low; Field; 2.35; Solid

The aim of this proposal is to expand the capability base that solid state NMR community has at its disposal so that more materials and chemistry systems can be effectively studied with this technique. Solid state NMR usually confines itself to the study of diamagnetic materials and compounds; i.e. systems that do not possess unpaired electrons in their electronic structure. Many modern materials and chemical systems being developed possess transition metals and/or rare earth species as part of the elemental composition; these introduce unpaired electrons into these systems and thus promote paramagnetic characteristics which are incompatible with the conventional NMR methodology. Our traditional mindset of how we approach the typical NMR measurement needs to be adjusted as our typical drive to higher external magnetic field strengths is counterproductive in this case. The electron polarisation that gives rise to paramagnetic anisotropies and shifts scales linearly with magnetic field, and these effects greatly detract from conventional NMR data thus masking the information that is normally sought. Severe cases of paramagnetism can preclude the NMR measurement of some systems completely.The most direct way to address this solid state NMR challenge is to attempt measurements in a much reduced (rather than increased) magnetic field, and to spin the sample at very high MAS frequencies. This low field/fast MAS methodology maximises the chance for NMR data to be elucidated from these systems, however these types of NMR spectrometers are very rare commodities worldwide. While many thousand NMR instruments exist throughout the world at fields of 7.05 T (300 MHz for 1H) and above, only a handful of operational low field spectrometers exist to undertake these type of measurements; furthermore, the UK is not well catered for in this field of spectroscopy apart from very limited proof-of-concept pilot studies that have demonstrated this idea. This new capability will be as easy to operate as conventional solid state NMR instrumentation and no specific additional training is required to enable its usage for data acquisition. The impact of this methodology is expected to influence the fields of catalysis and energy materials (battery materials, solid oxide and H conduction fuel cells, hydrogen storage materials, supported metal nanoparticles systems, zeolites, nuclear waste glasses etc.), general organometallc and inorganic chemistry, and the emerging field of medical engineering (rare earth doped biomaterials for oncology and blood vessel growth stimulation applications). It is also expected that this methodology will bridge across to established techniques such as EPR, and emerging technologies such as DNP, both of which employ different strategies for the manipulation of the paramagnetic interaction. These relationships are expected to stimulate a more vibrant magnetic resonance community that will be capable of collaboratively tackling the challenging research issues that confront the UK. Academic collaborators at Cambridge, Birmingham, Imperial, Queen Mary, Kent, UCL and Lancaster, and industrial partners such as Johnson Matthey and Unilever are all acutely aware of these new solid state NMR possibilities and flexibility that this methodology offers, and they eagerly await the improvements to the measurement technology that a low field/fast MAS combination can offer.The specific objectives that shape this proposal are:(a) to deliver a shared low-field/fast MAS solid state NMR resource to the UK magnetic resonance community that will augment the current UK suite of solid state NMR instrumentation in existence,(b) to put in place a state-of-the-art solid state NMR console and appropriate fast MAS probe technology capable of delivering the most modern experiments,(c) to align this methodology with established characterisation technologies such as EPR and emerging experimental initiatives such as DNP.

该提案的目的是扩大固态NMR社区所掌握的能力基础，以便可以通过该技术有效地研究更多的材料和化学系统。固态NMR通常局限于研究磁磁材料和化合物的研究。即，在其电子结构中不具有未配对电子的系统。开发的许多现代材料和化学系统都具有过渡金属和/或稀土物种，作为元素组成的一部分；这些将未配对的电子引入这些系统，从而促进与常规NMR方法不相容的顺磁性特征。在这种情况下，我们对典型的NMR测量方式进行典型的NMR测量的传统思维方式需要进行调整。引起顺磁各向异性并与磁场线性缩放的电子极化，这些效果极大地降低了常规的NMR数据，从而掩盖了通常所寻求的信息。严重的参磁性病例可以完全排除某些系统的NMR测量。应对这种固态NMR挑战的最直接方法是尝试在大量降低（而不是增加）磁场的测量中，并以非常高的MAS频率旋转样品。这种低场/快速MAS方法可以最大限度地利用NMR数据从这些系统中阐明，但是这些类型的NMR光谱仪在全球范围内非常罕见。尽管世界各地有数千名NMR仪器在7.05 t的田地上存在（1H及以上300 MHz），但只有少数几个操作的低场光谱仪可以进行这些类型的测量。此外，除了表现出这一想法的非常有限的概念验证试验研究外，英国在这一光谱学领域还没有很好地满足。这种新功能将像常规的固态NMR仪器一样易于操作，并且不需要其他额外的培训来实现其数据获取的用法。预计该方法的影响会影响催化和能源材料（电池材料，固体氧化物和H传导燃料电池，氢存储材料，支持的金属纳米颗粒系统，沸石，核废料玻璃等），一般有机分析和无机化学性能以及医学工程的无机化学领域（稀有的地球化学工程（稀有地球化的生物学生物学刺激）的刺激性刺激性和血液学）。还可以预期，该方法将介绍诸如EPR等既定技术，以及诸如DNP之类的新兴技术，这两种技术都采用不同的策略来操纵顺磁相互作用。预计这些关系将刺激一个更加活跃的磁共振社区，该社区将能够协作解决英国面临的具有挑战性的研究问题。剑桥，伯明翰，帝国，玛丽皇后，肯特皇后，UCL和兰开斯特的学术合作者以及诸如约翰逊·马特西（Johnson Matthey）和联合利佛（Unilever）等工业伙伴都敏锐地意识到这种方法学提供的这些新的固态NMR可能性和灵活性，并且他们急切地等待着一项特定的对象（均可提出的对象）。低场/快速MAS固态NMR资源向英国磁共振社区，该社区将扩大目前存在的固态NMR仪器套件，（b）建立一个最先进的固态NMR控制台和适当的快速MAS探针技术，能够提供最现代的实验，以使其与既定的实验效率相匹配，例如，（c）诸如诸如ERIND的eRning诸如eprient和e-eprient诸如Erprities诸如Erprities和Enpriend。

项目成果

The Impact of Intergrain Phases on the Ionic Conductivity of the LAGP Solid Electrolyte Material Prepared by Spark Plasma Sintering.

• DOI: 10.1021/acsami.3c03839
• 发表时间: 2023-08
• 期刊: ACS applied materials & interfaces
• 影响因子: 9.5
• 作者: Sorina Creţu;David G. Bradley;Liye Feng;O. U. Kudu;L. Nguyen;Tuan‐Tu Nguyen;A. Jamali;J. Chotard;V. Seznec;J. Hanna;Arnaud Demortière;M. Duchamp

In Situ Cross-Linking of Silane Functionalized Reduced Graphene Oxide and Low-Density Polyethylene

• DOI: 10.1021/acsapm.0c00115
• 发表时间: 2020-04
• 期刊: ACS Applied Polymer Materials
• 影响因子: 5
• 作者: S. S. Abbas-S.;Gregory J Rees;G. Patias;C. Dancer;J. Hanna;T. McNally

Cold sintering of bioglass and bioglass/polymer composites

生物玻璃和生物玻璃/聚合物复合材料的冷烧结

• DOI: 10.1111/jace.19022
• 发表时间: 2023
• 期刊: Journal of the American Ceramic Society
• 影响因子: 3.9
• 作者: Andrews J

Crystal Chemistry of Vanadium-Bearing Ellestadite Waste Forms.

• DOI: 10.1021/acs.inorgchem.8b01160
• 发表时间: 2018-07
• 期刊: Inorganic chemistry
• 影响因子: 4.6
• 作者: Yanan Fang;S. Page;Gregory J Rees;M. Avdeev;J. Hanna;T. White

Cysteamine functionalised reduced graphene oxide modification of maleated poly(propylene)

• DOI: 10.1016/j.polymer.2020.122750
• 发表时间: 2020-08-26
• 期刊: POLYMER
• 影响因子: 4.6
• 作者: Abbas, Syeda S.;Kelly, Nicole L.;McNally, Tony
• 通讯作者: McNally, Tony