Periodic Reporting for period 1 - ATMCinsituNMR (Next level real-time characterisation of Li- and Na-ion batteries by – Automatic Tuning Matching Cycler (plus Goniometer) – ATMC(+G) in situ NMR)
Reporting period: 2015-03-01 to 2017-02-28
OBJECTIVES: (a) Overcome experimental challenges of in situ NMR on LIB/NIBs, by designing a new NMR probe system and a highly shielded in situ cell attachment setup. (b) Perform ATMC in situ NMR on lithium iron phosphate (LFP) cathodes as well as their Na-ion based “counterpart”, sodium iron phosphate (NFP). Comparing the underlying chemistries based on the in situ NMR experiment should facilitate the development of cheaper NIBs as an accessible alternative to LIBs in the near future. (c) Apply the ATMC in situ NMR hardware to other (so-called) “beyond-Li” battery materials, including tin and Na-metal anodes for NIBs, as well as hard carbon electrodes. In addition, the new approach should be enhanced to study promising (but highly complex) sodium vanadium phosphate fluoride (NVPOF) cathodes for NIBs.
CONCLUSIONS: The design and application of the new hardware has been a great success and pushed forward the current state-of-the-art in real-time studies of LIBs/NIBs materials. Our ATMC in situ NMR system overcame all hardware issues that impaired such in situ investigations before. In addition, a new in situ cell design, the plastic cell capsule (PCC), has been developed, making a variety of battery materials amenable for in situ NMR. The approach was applied to numerous battery materials as detailed below. Furthermore, based on some parts of this new ATMC in situ NMR equipment, an additional hardware device was designed: the external automatic tuning/matching (eATM) ROBOT, which we subsequently applied in numerous NMR investigations of energy storage materials. This eATM ROBOT helped to increase the measurement efficiency and, by automating several experimental steps, significantly accelerated this aspect of battery research. The ATMC in situ NMR approach, in conjunction with the PCC, has been applied to the above-mentioned electrode materials. These investigations afforded deep insights into structure-property-relationships of these materials, which helped to understand their electrochemical performance.
FINDINGS: ATMC in situ NMR on LFP, NFP, and NVPOF cathodes offered insights into sructural changes of these materials during cycling. Furthermore, in situ NMR on Na-metal anodes helped to monitor the formation of different Na-metal species, and to quantify the electrolyte consumption during the electrochemical experiment. In addition, ATMC in situ NMR in combination with other experimental techniques provided insights into the structure of hard carbon anodes in NIBs.
EXPLOITATION/DISSEMINATION: The dvelopments/findings have been published in 8 scientific articles and 3 publications from conference proceedings. Furthermore, the research outcomes were disseminated in 13 talks and 6 poster presentations at conferences. The hardware developments have been made accessible the world-wide community of researchers via an industry partner. In addition, we reached out to the public at large, in particular to school children, through (hands-on) experiments on batteries made out of lemons; we discussed energy storage at a ""Scientific Lunch Break"" talk in 2015 and the ""Cambridge Science Festival"" in 2016. Furthermore, the objectives of this research have been explained to the public in an interview (press release; print and online) with the ""Cambridge News"" as well as an ""Instagram feature"" in 2016."