Jeol Ltd.
Jeol Ltd.
02/04/2026 | Press release | Distributed by Public on 02/03/2026 19:53
Operando Battery Probe [Application Notes]
In the field of battery material development, NMR spectroscopy is a vital tool for the direct observation of Li and Na nuclei, providing detailed information on local structures and reaction processes. Our operando battery NMR probes allow for the real-time monitoring of structural changes during charge-discharge cycles, offering valuable insights into the electrochemical behavior of materials under actual operating conditions.
Operando Battery Probe
Operando NMR Cell
Pseudo Goniometer
The Operando NMR cell allows angle adjustment in four steps: 0°, 30°, 60°, and 90°.
Changing the sample's angle relative to the magnetic field is useful for obtaining orientation information and identifying signals. The figure on the right shows the angle dependence of the signals from the Li electrode and Li dendrites. Since both signals originate from Li metal, they appear close to each other; however, Li dendrites consist of needle-like metallic Li structures several micrometers in size that grow in various directions relative to the magnetic field, whereas the electrode exhibits a strong angle dependence because only surface signals are detected due to the skin effect. As a result, the electrode signal shows a larger angular dependence.
Example 1: Operando Observation of Lithium Dendrites
NMR is the only analytical technique capable of distinguishing Li dendrites from Li species in electrolytes or active materials. By using the operando battery probe, the formation and disappearance of dendrites inside a battery can be monitored in real time. Here, the generation of dendrites caused by overcharging is observed by 7Li operando NMR measurements. The dendrite signal appears at around 270 ppm due to the Knight shift. The cell used in this experiment is a Li symmetric cell in which both electrodes are composed of Li metal. Although the Li electrode signal also appears near this region because of the Knight shift, the signals originating from the dendrites and the electrode can be distinguished, as they appear at different positions owing to their different orientations relative to the magnetic field.
Sample: Li symmetric cell
Li / glass filter / Li
Current collector: Cu
electrolyte: 1 M LiPF6/ EC+ DMC (3:7 v/v) 60µL
Measurement condition
ECZL-500G
7Li 90 pulse width = 12us
Frip angle =45 deg
Relaxation delay =5s
Scans =8 / 1 spectrum
Example 2 : Operando Observation of Li ion Intercalation/Extraction in Graphite
Graphite is the most commonly used layered compound for the anode material in lithium-ion batteries due to its low potential and high stability. During charging, Li is inserted into the interlayer spaces, while during discharging, it is deintercalated. Operando measurements make it possible to observe, in real time, the insertion and extraction of Li in graphite during charge-discharge processes. Here, 7Li operando NMR spectra of a half-cell using a Li metal counter electrode are shown. In the half-cell configuration, the Li electrode serves as the anode and graphite as the cathode, because lithium has a lower potential. During discharge, a signal originating from Li inserted into graphite appears at around 40 ppm. During charging, this signal disappears and a new signal emerges at approximately 250 ppm. These observations indicate that Li is deintercalated from the graphite and deposited onto the Li electrode during charging.
Sample: Li graphite half cell
Li-Graphite half cell
Li / glass filter / Graphite:PVdF=90:10 (w/w)
Current collector: Cu
electrolyte: 1 M LiPF6 / EC+ DMC (3:7 v/v) 120µL
Measurement condition
ECZL-500G
7Li 90 pulse width = 12us
Frip angle =45 deg
Relaxation delay =5s
Scans =256 / 1 spectrum
Courtesy of Dr. Yuta Ito (AIST) for sample preparation and measurement support
Solutions by field
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