The battery research and production process

Thermo Scientific systems touch every part of the battery value chain, from extraction and processing of raw materials, to quality assurance in the production line, to research and development of new battery designs.

Battery research applications

Selected use cases for battery research

Challenge

Technologies

Solution

Resources

Avoid contamination of air-, moisture-, and/or beam-sensitive battery samples during preparation and sample transfer

IGST workflow:

DualBeam, SEM/Desktop SEM (in glove box), TEM, Avizo, CleanConnect

Complete workflow to enable sample characterization of sensitive battery materials in their native state without contamination

Brochure: Seamless inert gas sample transfer workflow

Datasheet: CleanConnect Sample Transfer System

App note: Benefits of the Phenom XL G2 Desktop SEM's argon compatibility for lithium battery research

Detection of lithium is difficult using SEM, EDS, and TEM

TOF-SIMS

Accurately detect and map lithium in battery samples in 2D and 3D down to 10 ppm

App note: Ion spectroscopy using TOF-SIMS on a Thermo Scientific Helios DualBeam

TEM

iDPC technology can clearly image light elements like lithium at atomic scale

App note: Integrated Differential Phase Contrast on Talos S/TEM

Characterize battery structure at different scales beyond the capacity of a single instrument

CT, SEM, Raman, DualBeam, Avizo, EDS

Correlative workflow allowing multiscale imaging and analysis of battery microstructure

App note: Multiscale image-based control and characterization of lithium-ion batteries

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

Prepare a large 2D area on the sample surface with high polishing quality for 2D imaging and characterization

DualBeam (Plasma FIB-SEM), EDS

High-throughput automated spin mill with high surface quality

App note: Large area automated sample preparation for batteries

SEM, CleanMill

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

Characterize key microstructure properties (like tortuosity) for electrode structure performance correlations

DualBeam, EDS, TOF-SIMS, Avizo

3D characterization of battery structure

·    Hardware to image 3D battery structure at different scales

·    Software to automate 3D imaging data collection

·    Thermo Scientific Avizo Software workflow for image analysis and quantification

Blog post/video: Advancing lithium-ion battery technology with 3D imaging

App note: Multiscale image-based control and characterization of lithium-ion batteries

Characterize beam-sensitive materials like SEI at nanoscale

TEM, EDS, Avizo

Nano- and atomic-scale characterization of energy materials

·    Cryo-EM workflow for accurate data collection with superior EDS performance

·    Avizo Software for structure quantification and visualization

Brochure: Analytical solutions for battery and energy storage technology

Webinar: Cryo- and in situ electron microscopy diagnosis-guided design of rechargeable battery materials for better batteries

Webinar: Advanced characterization methods of electrochemical materials and interphases for better batteries

In situ kinetic analysis (like heating) via electron microscope

SEM

Multiple in situ heating stage choices with integrated software for Thermo Scientific SEMs to understand cathode synthesis mechanisms

Brochure: Scanning electron microscopy for lithium battery research

Characterize beam-sensitive separator samples without damage

SEM/SDB

Superior low-KeV imaging and a cryo-FIB milling solution allow characterization of separator microstructure in 2D and 3D

App note: Strategies for accurate imaging on battery separator structure

Probe intrinsic SEI within a coin cell via electron microscopy

Laser Plasma FIB

High-energy, high-milling rate laser enables direct cross-section milling to understand Li-metal cell degradation mechanism

Webinar: Visualizing Li-metal anode battery degradation

Understand stoichiometry of solid electrolyte film as a function of depth

XPS

XPS depth profiling can quantify elements at each depth

 

Webinar: Understanding surface reactions of the solid electrolyte interface via advanced characterization techniques

Measure electrode surface chemistry

XPS

XPS can quantify the chemical states present at the electrode surface

App note: Analysis of electrode materials for lithium ion batteries

Track the evolution of the SEI layer

XPS

Materials can be depth profiled using XPS and a cluster ion source to follow the development of the SEI layer after cycling

 

In situ electrode cycling

XPS

Electrodes can be operated in situ to monitor spectral changes as they are charged and discharged

 

Investigate changes in separator chemistry during cell lifetime

XPS

The surface chemistry of polymeric materials is easily characterized using XPS

 

Profile battery components ex situ without missing point-to-point variability across an area

Raman

Raman microscopy can be used to look at changes to materials and distributions of components that occurred during use or testing

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

Identify phases and determine structures in anodes and cathodes

Raman

Raman microscopy can visually show the spatial distribution of different phases of the same material with different performance characteristics

App note: Raman analysis of lithium-ion batteries – Part I: Cathodes

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

XRD

XRD can help to identify and quantify specific polymorphic structures of interest to increase yield and efficiency

Brochure: ARL EQUINOX 100 X-ray Diffractometers

Trace and map anode composition across charge and discharge cycles

Raman

Raman microscopy can be used for in situ monitoring of changes on electrode surfaces during charge/discharge cycles

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

Confirm the presence of specific carbon allotropes as anode components and in hybrid materials

Raman

Raman spectroscopy is particularly adept at the analysis of allotropes of carbon, including carbon in hybrid materials

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

Understand the association of ionic species and distribution of components in solid polymer electrolytes (SPEs)

Raman

Raman microscopy can be used to visualize the spatial distribution of components in SPEs and indicate ionic associations

App note: Raman analysis of lithium-ion batteries – Part III: Electrolytes

Study crystallinity, stability, and reactivity in battery materials

XRD

X-ray diffraction can determine the percentage of crystallinity vs amorphous content of the active material, as well as structural stability and repeatability in real time

Brochure: ARL EQUINOX 100 X-ray Diffractometers

Follow charge/discharge reactions in situ

XRD

During charge/discharge, the cathode and anode of every battery cell undergo changes. XRD allows you to follow the changing phase composition and the evolution of the crystalline structure

Webinar: Drill down to microstructures with XRD

Abbreviations: Avizo = Avizo Software; CT = Computed tomography; DualBeam = Focused ion beam scanning electron microscopy (FIB-SEM); EDS = Energy-dispersive X-ray spectroscopy; FIB = Focused ion beam; FTIR = Fourier transform infrared spectroscopy; iDPC = Integrated differential phase contrast; IGST = Inert sample gas transfer; SDB = Small DualBeam; SEI = Solid electrolyte interface; SEM = Scanning electron microscopy; SPE = Solid polymer electrolytes; TEM = Transmission electron microscopy; TOF-SIMS = Time of flight secondary ion mass spectrometry; XPS = X-ray photoelectron spectroscopy; XRD = X-ray diffraction.


Battery mineral resource processing

Selected use cases for battery mineral processing

Challenge

Technologies

Solution

Resources

Elemental analysis and grade control of nickel, cobalt, manganese, iron, lithium ores

XRF

Thermo Scientific XRF lab spectrometers can quantify up to 90 elements in liquid or solid samples of mining materials, enabling control of ore body content for refinement and processing

App note: Analysis of Nickel Ore with ARL OPTIM'X WDXRF Spectrometer

App note: EDXRF Analysis of Nickel Ore as Pressed Powders in an Air Environment

App note: Analysis of lithium raw materials with WDXRF
App note: Manganese ore analysis with the ARL OPTIM’X XRF Spectrometer 
App note: Iron ore analysis with the ARL OPTIM’X XRF Spectrometer

Abbreviations: XRF = X-ray fluorescence.


Battery raw materials control

Selected use cases for battery raw materials control

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

Abbreviations: EDS = Energy-dispersive X-ray spectroscopy; FTIR = Fourier transform infrared spectroscopy; ICP = Inductively coupled plasma; OM = Optical microscopy; SEM = Scanning electron microscopy; XRD = X-ray diffraction; XRF = X-ray fluorescence.


Battery production applications

Selected use cases for battery production

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.

Twin-screw Extrusion

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

On-demand webinar: Compound homogeneous electrode slurries fast and effectively

Abbreviations: DualBeam = Focused ion beam scanning electron microscopy (FIB-SEM); EDS = Energy-dispersive X-ray spectroscopy; FIB = Focused ion beam; ICP = Inductively coupled plasma; NCM = Nickel cobalt manganese; OES = Optical emission spectrometry; OM = Optical microscopy; SEM = Scanning electron microscopy.


Battery quality control

Selected use cases for battery QA/QC

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: Small spot analysis: Performance in ferrous base

App note: Sample analysis using elemental mapping at low power with Thermo Scientific ARL PERFORM’X 1500 W Advanced WDXRF Spectrometer

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.
Rotational Rheometry Characteristic flow curves (the slurry viscosity over shear rate) provide insight of the slurries' flow behavior in processes like pumping, stirring, and coating.  Thermo Scientific HAAKE iQ Air Rotational Rheometers are used to measure flow curves over a broad range of shear rates with high precision. On-demand webinar: Rotational Rheology in Battery Manufacturing and Research

 

Abbreviations: DualBeam = Focused ion beam scanning electron microscopy (FIB-SEM); EDS = Energy-dispersive X-ray spectroscopy; FIB = Focused ion beam; ICP = Inductively coupled plasma; NCM = Nickel cobalt manganese; OES = Optical emission spectrometry; OM = Optical microscopy; SEM = Scanning electron microscopy.


Battery recycling

Selected use cases for battery recycling

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.

App note: Analysis of traces in graphite

Abbreviations: EDS = Energy-dispersive X-ray spectroscopy; ICP = Inductively coupled plasma; OM = Optical microscopy; SEM = Scanning electron microscopy; XRF = X-ray fluorescence.