Materials, Parameters and Methods to Analyze Batteries: Battery Research

Battery research entails the development process from concept and theory validation of new materials to the quality control and characterization of raw materials and finished batteries.

Progress in the pursuit of higher energy, power density, and more efficient energy storage is dependent on sophisticated instrumentation for the characterization of cells and materials. To enable and support your research, Metrohm supplies the user with top-quality analytical instruments, know-how, and superior on-site service.

The parameters of interest and which method can be used to analyze them with Metrohm instrumentation are detailed in the table below.

Source: Metrohm AG 

Sample Parameter of
interest
Analysis
technique
Metrohm
Application
Documents
Anode
(raw materials)
Water content Karl
Fischer titration
AB-434
Eluated anions and cations Ion
chromatography
 
Cathode
(raw materials)
Purity of lithium salts (LiOH, Li2CO3, LiNO3, LiCl) Titration AN-T-215,
AN-T-216,
AN-T-181
Impurities in lithium salts (e.g., sodium, ammonium) Ion
chromatography
AN-C-189
Ni, Co, Mn content in solution for cathode material production (single metal or mixture) Titration,
Voltammetry
AN-T-218
Cobalt, nickel, iron, manganese in various cathode material  Titration  
Water content Karl
Fischer titration
AB-434
Eluated anions and cations Ion
chromatography
 
Through-plane tortuosity Electrochemistry AN-BAT-011
Electrolytes, electrolyte additives and electrolyte solvents Water content Karl Fischer titration AB-434
Cations and anions in electrolyte (e.g., LiPF6) Ion
chromatography
AN-C-037,
AN-CS-011,
AN-N-012
Decomposition products of LiPF6 Ion
chromatography
AN-S-372
Electrolyte resistance Electrochemistry  
Solid electrolyte interface investigation Electrochemistry AN-BAT-010
Diffusion coefficient Electrochemistry AN-BAT-009
Lithium ion transference number Electrochemistry AN-BAT-012
HF content in electrolyte Titration  
Separators Water content Karl Fischer titration AB-434
Eluated anions and cations Ion
chromatography
 
MacMullin number Electrochemistry AN-BAT-006
Finished
batteries
Voltage characteristics upon charge and discharge Electrochemistry AN-BAT-001,
AN-BAT-002
Cycling performance and coulombic efficiency Electrochemistry WP-052
Cycle and calendar life evaluation Electrochemistry  
Battery capacity and power Electrochemistry  
State of charge, depth of discharge and state of health Electrochemistry  
Internal battery resistance Electrochemistry  
Charge transfer resistance Electrochemistry  
Diffusion coefficient (GITT and PITT) Electrochemistry AN-BAT-003,
AN-BAT-004
Eluated anions and cations Ion chromatography    

 

Analysis Methods

Electrochemistry – Ideal for Studying the Performance of Batteries and Battery Materials

Image Credit: Metrohm AG

Electrochemistry – Ideal for Studying the Performance of Batteries and Battery Materials

The specially designed potentiostats/galvanostats from Metrohm are employed for the characterization of battery raw materials, in addition to finished batteries. Electrochemical measurements are based on highly accurate control and measurements of electrical charge, voltage, impedance, or current.

Voltammetry is a highly sensitive technique that has LODs in the ppb range. It can be utilized for the analysis of electrochemically active substances, like organic or inorganic ions.

For instance, voltammetry enables the simultaneous determination of cobalt, nickel, and manganese in cathode materials. This method can be combined with a large variety of applications and has short analysis times and high precision with comparatively low costs of the instrumentation required.

Titration – Specific, Accurate and Reliable

Image Credit: Metrohm AG

Titration – Specific, Accurate, and Reliable

Potentiometric titration is ideally suited for establishing the purity of lithium salts or metals which are employed in cathode materials, like cobalt, iron, manganese, or nickel. It is applied to analyze standard solutions utilized for the preparation of cathode materials or finished cathode materials.

Titration does not require dilution of such samples, unlike competing techniques such as ICP-MS or AAS, so the results which are gathered by titration are more accurate and reliable. Compared with ICP-MS or AAS, Maintenance and running costs are also considerably lower.

Karl Fischer Titration – The Preferred Method for Water Determination

Image Credit: Metrohm AG

Karl Fischer Titration – The Preferred Method for Water Determination

As water reacts with the conducting salt, e.g., LiPF6, to form hydrofluoric acid, lithium-ion batteries must be totally free of water (concentration of H2O < 20 mg/kg).

For establishing water content at trace levels, sensitive coulometric Karl Fischer titration is the perfect technique. For solids, water determination is performed by utilizing the Karl Fischer oven technique. This is where residual moisture in the sample is evaporated and transferred to the titration cell, where it is subsequently titrated.

Ion Chromatography – Highly Efficient Multi-Parameter Analysis of Electrolytes and Metals Salts

Image Credit: Metrohm AG

Ion Chromatography – Highly Efficient Multi-Parameter Analysis of Electrolytes and Metals Salts

Ion chromatography (IC) is a precise and efficient multi-parameter technique that can be used to quantify decomposition products in electrolytes, impurities in lithium salts, and anions and cations in eluates of numerous battery raw materials.

This information has been sourced, reviewed and adapted from materials provided by Metrohm AG.

For more information on this source, please visit Metrohm AG.

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