The solid-state NMR platform at CIC energiGUNE is composed by state-of-the-art equipment specially designed for the analysis of energy storage materials including batteries, supercaps and thermal energy store materials also by ex situ and in situ methods. We have a long record of publications, industrial projects and international collaborations in these fields. In particular, our platform is composed by:

1. WB BRUKER AVANCE III 500 MHZ

The Avance III 500 MHz was installed at CIC in April 2012. It is a wide bore magnet especially suited for non magnetic materials where high resolution is desired.

WB This high field spectrometer is designed for the characterization of solid materials for electrochemical energy storage applications. Including anode, cathodes, ceramic and polymer-based solid electrolytes and supercaps. These materials can be studied ex-situ and in-situ using a custom-made probehead that is not accessible in common solid-state NMR laboratories. Our areas of expertise include the structural characterization of battery materials, the understanding of the degradation mechanisms and post-mortem analysis of batteries and supercaps, the understanding of the key parameters involved in the observed electrochemical performance and the kinetic processes of Li+ and Na+ diffusion.

The materials investigated include ceramics, polymers, metals and alloys, porous materials, biologic materials and composites. All these areas are open to external users. The in-situ system is the phase of testing and implementation and is expected to be available to external users by March 2021.

In the area of thermal energy storage, our platform is equipped with variable temperature probes that allow the in-situ characterization of phase transitions in organic and inorganic materials up to 200C.

Available Probes:

• Double resonance 1H/19F-X DVT CPMAS 1.3 mm probe that can reach ultra-fast spinning speeds of up to 67 kHz

• Triple resonance 1H-X–Y, DVT CPMAS 2.5 mm probe that can spin up to 35 kHz

• Static wideline H-X probe for variable temperature studies

• Variable temperature measurements between 300ºC and -100ºC

2. WB BRUKER AVANCE III 200 MHZ

The Avance III 200 MHz was installed at CIC in March 2012. It is a wide bore, low magnetic field magnet dedicated to the study of paramagnetic materials which are a frequent component in battery and supercapacitor electrodes.

This low field solid state NMR spectrometer is specially designed for the characterization of paramagnetic materials that are used as cathode electrodes. This magnet combines a rather low magnetic field with a very fast MAS probe of 1.3 mm rotors allowing Magic Angle Spinning (MAS) frequencies of up to 67 kHz.

This setup is rather unique and is essential for the accurate characterization of cathode materials. We have a very strong background of high impact publications in this field and we are among the few solid-state NMR platforms that are able to perform such measurements worldwide.

Available Probes:

• Double resonance 1H/19F-X DVT CPMAS 1.3 mm probe that can reach ultra-fast spinning speeds of up to 67kHz.

• Double resonance 1H-X DVT CPMAS 4 mm probe, that can reach temperatures up to 400ºC and spinning speeds up to 18 kHz.

• Variable temperature measurements between 400ºC and -100ºC.

Our solid-state NMR platform was officially recognised in 2018 by Bruker-Spain as the reference centre for solid state NMR in Spain. Our platform combines state of the art hardware and software capabilities with a highly qualified human resources for the experimental design and deep analysis of the solid-state NMR

data.