Battery Research and Manufacturing Applications

Challenge

Technologies

Solution

Resources

Electrode materials QC requires higher resolution than OM, but floor-based SEMs won’t fit in our lab and manual analysis is too slow

Desktop SEM

The Thermo Scientfic Phenom XL Desktop SEM can handle high-resolution morphology analysis and QC of anode and cathode materials with high-throughput automation

Blog post: Analysis of graphite for lithium-ion batteries

Identification and quantification of metal impurities in raw materials is critical, but neither ICP nor optical microscopy does both

Desktop SEM, EDS

Thermo Scientfic Phenom ParticleX Desktop SEM can identify and quantify particle impurities with high-throughput automated EDS workflow

Webinar: How to certify your NCM powder quality with SEM+EDS

Rapidly characterize lithium, metal oxide, and lithium compounds

Raman

Thermo Scientific Raman instruments can analyze these compounds quickly with minimal sample preparation

Blog post: Using Raman spectroscopy during lithium-ion battery manufacturing

Characterize lithium and other highly reactive salts

FTIR

Compact Thermo Scientfic Nicolet FTIR instruments can measure sample spectra within an argon-purged glove box using remote control

App note: FTIR characterization of lithium salts in an inert atmosphere

Characterize raw materials

XPS

XPS can be used to analyze the surface of powdered materials prior to formation of electrodes, determining stoichiometry and identifying contaminants

Evaluate purity of raw materials

XRF

Elemental analysis from ppm to 100%, pre-screening for impurities in carbon black

Brochure: X-ray Product Range

Identify and quantify mineral composition in raw materials

XRD

Phase identification and structure determination in anode and cathode

Brochure: ARL EQUINOX 100 X-ray Diffractometers

Challenge

Technologies

Solution

Resources

Detection of electrode impurities is slow and tedious using normal SEM-to-EDS workflow

ChemiSEM, EDS

Thermo Scientfic Axia ChemiSEM integrates SEM with “live EDS” for immediate characterization of electrode impurities

App note: Assessment of contaminants within battery materials via Axia ChemiSEM

Failure analysis and QC in battery production requires SEM-level resolution, but floor models take too much space

Desktop SEM

Phenom Desktop SEMs enable high-resolution, high-throughput analysis of battery materials

App note: Investigate batteries with a SEM for better performance

Identification and quantification of metal impurities in raw materials is critical, but neither ICP nor OM does both

Desktop SEM, EDS

Phenom ParticleX Desktop SEM can identify and quantify particle impurities with high-throughput automated EDS workflow

Webinar: How to certify your NCM powder quality with SEM+EDS

Binder characterization is difficult but crucial to confirm electrode mechanical structure

SEM, DualBeam

Superior imaging contrast of unique T3 detector for Thermo Scientfic Apreo 2 SEM enables mapping of non-conductive binder distribution within electrode

Brochure: Scanning electron microscopy for lithium battery research

Simultaneously quantify major elements (% level) and trace impurities (ppm, mg/kg) of a battery cathode

ICP-OES

Thermo Scientfic iCAP 6000 Series ICP-OES can accurately measure concentrations in solutions ranging from <0.006 mg/L to nearly 3000 mg/L (6 orders of magnitude)

App note: Simultaneous determination of impurities and major elements in lithium-ion battery cathodes using the Thermo Scientific iCAP 6000 Series Radial ICP-OES

Battery slurries mixed batchwise in planetary mixers is labor-intensive, has low material efficiency, and bears the risk of batch-to-batch variations.

Electrodes coated by solvent-casting methods requires energy consumptive solvent evaporation and recycling techniques. Volatile solvents are hazardous and expensive.

Continuous slurry compounding reduces material loss, cleaning time, handling errors, and product variations.  Thermo Scientific twin-screw extruders continuously compound slurries with high reproducibility.

Control composition, material shear, and temperatures.

PTFE acts as a binder in solvent-free electrode slurries.  Compounding of PTFE and active material powders requires high shear.  Thermo Scientific twin-ccrew extruders successfully compound PTFE and active material to produce solvent-free slurries.  High shear renders formation of PTFE fibrils binding active material grains

Challenge

Technologies

Solution

Resources

Identification of impurities for root cause analysis is difficult using CT alone

CT/SDB, EDS, Avizo

A correlative CT/laser PFIB workflow can identify deeply embedded impurities without disassembling the cell

App note: Multiscale 3D imaging solutions for Li-ion batteries

Failure analysis requires high-resolution cross-section polishing while still protecting sample

SEM, CleanMill

Thermo Scientfic CleanMill offers a dedicated workflow for air-sensitive samples, an ultra-high energy ion gun for fast polishing, and a cryogenic function to protect sample integrity

Datasheet: CleanConnect Sample Transfer System

Differentiate carbon allotropes, reveal anode material structure, and track changes during usage

Raman

Raman spectroscopy is particularly useful for distinguishing between different allotropes of carbon and evaluating the structural quality of these materials

App note: Raman analysis of lithium-ion batteries – Part II: Anodes

Map degradation of the anode SEI layer

Raman

Raman microscopy can be used for visualizing changes to electrode materials and component distributions after a cell has been used

App note: Ex situ Raman analysis of Li-ion batteries

Monitor battery off-gassing or chemicals released during a fire, short circuit, or other hazardous conditions

FTIR

Thermo Scientfic Antaris IGS system with Heated Valve Drawer can quantify release of HF and other fluorinated gasses under overtaxed conditions like a vehicle crash

Tech note: Gas-phase FTIR for smoke toxicity measurements

Assess crystallinity, stability, and reactivity in battery materials

XRD

Check crystal structure, crystallinity, orientation characteristics, thickness, homogeneity, and density of thin films and layers

Brochure: ARL EQUINOX 100 X-ray Diffractometers

Detect defects, inclusions, and imperfections

XRF

Elemental mapping and small spot analysis down to 0.5 mm

App note: Sample analysis using mapping with ARL PERFORM’X Series XRF spectrometers

Control the purity of anodes, cathodes, electrolytes, separators, and other components

XRF

Wavelength dispersive X-ray fluorescence (WDXRF) allows routine, daily monitoring and control of impurities and contamination

App note: Analysis of traces in graphite

Quantify trace elements in lead and lead alloys according to current standards for lead-acid batteries

OES

The Thermo Scientfic ARL iSpark Optical Emission Spectrometer enables trace and alloying element analysis in lead-acid batteries

Analysis of lead and its alloys with the ARL iSpark OES spectrometer

Understanding the rheological properties of an electrode slurry is necessary to:

• Optimize the coating process
• Define the storage handling
• Characterize the quality of dispersion as a predictor for cell performance.

Challenge

Technologies

Solution

Resources

Recycled materials QC requires higher resolution than OM, but floor-based SEMs won’t fit in our lab and manual analysis is too slow

Desktop SEM

The Phenom XL Desktop SEM can handle high-resolution QC of recycled battery materials with high-throughput automation

Identification and quantification of metal impurities in recycled materials is critical, but neither ICP nor OM does both

Desktop SEM, EDS

The Phenom ParticleX Desktop SEM can identify and quantify particle impurities with high-throughput automated EDS workflow

Webinar: How to certify your NCM powder quality with SEM+EDS

Sort incoming materials to be recycled and control impurities in recovered metals

XRF

Black mass elemental analysis for recovery of metals, such as aluminum, nickel, cobalt, manganese and graphite.