Battery Testing and

Materials Characterization
A Selection Guide for Analytical Solutions

© 2023 TA Instruments. A division of Waters Corporation. All rights reserved.

1
Table of Contents

Full battery cell page 5

Battery Materials 6

• Electrodes 6

• Binder and additive 8

• Separators 11

• Electrolytes 13

Module Pack Materials 15

Technique Cheat Sheet 17

 Unlocking the Full Potential of Batteries
Cutting-Edge Analytical Solutions for the Next Generation of Battery Development

The race for the next generation of battery technology is well underway. In just a few decades, rechargeable batteries have
grown well beyond their roots in consumer electronics and now support sustainable transportation and renewable energy
storage. Tremendous advancements in battery efficiency, power, output, and safety have primed batteries, especially lithium-
ion batteries, for these demanding applications.

Now, battery developers are tasked with optimizing their designs for both current and new applications. In addition to building
safer, low-cost electric vehicles, batteries must reach even higher energy density for use in freight trucks and buses. Similarly,
batteries with higher capacity and lower costs will be the formulations of choice for grid energy storage. And above all else,
battery developers must meet demand for sustainable, affordable material sourcing in the face of lithium and cobalt scarcity.

The frontier for battery innovation is vast but the challenges are steep. Success will be determined by small margins in energy,
power output, cycle life, safety, and cost – all of which require superior optimization of battery materials and electrochemical
reactions. Leading labs rely on TA Instruments for analytical characterization and testing of their batteries.

Using the right techniques and instruments gives you the upper hand in efficiently advancing battery technology with proven
quality and performance. From R&D and material selection to manufacturing and quality control, TA Instruments’ solutions
support the full breadth of battery innovation. This guide explains our comprehensive battery offerings by battery component,
so you can find the right technique to enhance your battery development.

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 Cathode Manufacturing Binder & Additive
• Slurry viscosity and • Incoming materials QC Cathode Materials
coating performance • Verify materials • High temp stability
• Slurry structure and • Degradation • Sintering process
conductive network • Melting temperature
Electrodes

Anode Manufacturing Binder & Additive

• Slurry viscosity and • Incoming materials QC
coating performance • Verify materials
• Slurry structure and • Degradation
conductive network • Melting temperature

Battery Separators
Materials • Incoming materials QC Mechanical Integrity
• Verify materials • Thermal sinkage
• Degradation • Modulus
• Composition • Creep
• Inorganic coating content
• Melting temperature

Electrolytes Solvent based

Battery Applications

• Incoming materials QC
• Verify materials Gel Polymer Electrolytes
• Degradation • Viscoelasticity
• Composition • Gel point
• Melting temperature
• Glass transition temp

Thermal Adhesive Adhesive

• Degradation Thermal Adhesive • Curing
• Curing • Thermal conductivity • Viscoelasticity
• Glass transition temp
Module Pack
Materials
Casing
• Degradation Casing/Packaging Materials
• Composite content • Modulus
• Melting temperature • Glass transition
• Glass transition temp

Full Battery
• Cell Discharge
Full Battery • Heat capacity
HR Rheometer
• Parasitic reaction
Cell • Decomposition analysis
TGA and DSC
• Lithium Plating
• SEI formation
TMA/DMA

SDT

Thermal Conductivity

TAM

© 2024 TA Instruments. A division of Waters Corporation. All rights reserved.

4
 Full Battery Cell
Testing battery cells is an important step in optimizing battery chemistries and evaluating changes before scaling designs
to larger formats. Battery scientists need to determine cells’ efficiency as well as degradation during cycling.
When isothermal microcalorimetry (IMC) is paired with a cycler or potentiostat, critical insights on lifetime predictions, cell
performance rankings, and heat management evaluation can be developed.

Numerous notable battery labs, including the Jeff Dahn group and 3M,
have published research using TA Instruments isothermal microcalorimeters
paired with battery cyclers for full cell testing. The new Battery Cycler
Microcalorimeter Solution is built with this application in mind. The
solution pairs TA Instruments’ state-of-the-art TAM IV Microcalorimeter
to measure the thermal behavior of samples with the BioLogic VSP-
300 Potentiostat, a research-grade electrochemical analysis tool to
probe the electrical properties of materials. The result is an end-to-end,
in-operando measurement tool for elucidating the thermodynamic and
electrochemical details of battery cells in real time, in a flexible and intuitive
system with pre-programmed methods.

Method Description

Measures heat flow during cycling, primarily used for thermal management applications.
Heat Management (CCCV) This method will program different charging profiles (variable charge / discharge rates)
using constant current constant voltage (CCCV) parameters.

This method consists of a slow cycle (C/20) followed by a very slow cycle (C/100) for maximum
Entropy Changes
resolution into the structural and phase changes that occur during lithiation/delithiation.

Method designed to study the SEI formation reactions. This method applies a small charging
First Cycle Reaction
current in the low voltage range where SEI formation occurs (typically below 3.0 V), then applies
(SEI formation)
a higher charging current until the standard upper voltage limit is reached (typically 4.2 V).

Method to measure the parasitic power over the full voltage range. The term “parasitics” is a
Full Cycle Parasitics
blanket term for any non-reversible side reaction that contributes to battery degradation.

Method to measure the parasitic power in a narrow voltage.

Narrow Cycle Parasitics
This is a faster technique if only one (or more) narrow voltage windows are of interest.

Experiment for measuring the self-discharge rate. This combines the conventional technique
Self-Discharge (monitoring open circuit voltage over time, then discharging to measure the remaining capacity)
and the thermal method of integrating the total heat produced over the open circuit time.

Custom experiments, programmed by selecting actions, wait times, and event markers
Manual
in the run sequence menu.

Battery Cycling Resources

Application Note: Determination of Parasitic Power in Lithium-ion Batteries using the Battery Cycler Microcalorimeter Solution

Application Note: An Overview of Isothermal Microcalorimetry in Battery R&D and QA - TA Instruments

Learn more about the Battery Cycler Microcalorimeter Solution.

5
 Battery Materials
Electrodes
Electrodes connect battery terminals to the electrolyte and house the chemical reactions for charging and discharging.
Electrodes therefore must demonstrate good electrochemical stability with the electrolyte as well as hold large amounts of
ions without changing their structure. Cathode materials have been at the forefront of battery innovation in recent years, with
anode materials now gaining attention as the next area of development.

Electrode Manufacturing
All batteries require cathode and anode coatings on a current collector. Modern industrial battery manufacturing uses slot-
die coating, in which the electrode slurry is deposited onto the current collector to form a smooth, uniform coating. In order
to speed up battery manufacturing, researchers are optimizing slurry formulations and testing different drying temperatures.

Rheology enables engineers to produce consistent slurry viscosities that result in uniform coatings for high performing and
safer batteries. A rheological profile measurement can help ensure a uniform, defect-free coating that leads to production of
consistent, high-quality electrodes with high batch-to-batch repeatability and low scrap rates. Engineering new slurry materials,
formulations, or processing methods all require thorough rheological characterization to verify the slurry’s quality.

Using accurate, reliable rheometers gives labs the upper hand in predicting slurry behavior before application, saving
valuable resources and time. Screening incoming raw materials or new formulations helps users detect unexpected behavior
and avoid large-scale production issues. While viscometers measure basic viscosity and flow, rheometers add shear or stress
measurements that provide crucial information on slurry structure and behavior.

What to Measure Technique What it Means Why it Matters TA Instrument

The stability and shear-rate

Optimize coating speed
Viscosity Rheology dependent flow behavior Discovery HR
and electrode quality
of a slurry

Whether the slurry is

Identify slurry
Viscoelasticity Rheology liquid-like or gel-like at Discovery HR
network structure
different frequencies

Determine shelf life

Minimum stress required and stability against
Yield Stress Rheology Discovery HR
to initiate a flow sedimentation or phase
separation

Measure the coating Choose the most cost-

Drying Time TGA Discovery TGA
drying time and kinetics effective drying process

Determine slurry structure

Thixotropy and Thixotropic A time-dependent shear change during coating
Rheology Discovery HR
Recovery thinning phenomenon and recovery of the
structure

Ensure optimal
Shear-dependent Discovery HR
Impedance Rheo- conductive network
conductive network and Rheo-Impedance
under Shear Flow Impedance under the relevant
structure change Spectroscopy
processing conditions

© 2024 TA Instruments. A division of Waters Corporation. All rights reserved.

6
 The ideal slurry has a low viscosity for optimum mixing
and coating (high shear rates), but a high enough
viscosity for good levelling during drying and for
minimizing particle settling and agglomeration during
storage (low shear rates).

Since slurries are made up of solid particles of active

materials, conductive additive, polymeric binder, and
solvent, battery labs benefit from rheometers capable
of testing all materials separately as well as combined
in a slurry. The Discovery Hybrid Rheometer is uniquely
capable of switching between solid, liquid, and
powder samples in less than 10 seconds with industry-
leading results and intuitive operation.

ed Peltier Pl
v a nc ate
Ad

centric Cy
r Con lind
ltie er
Pe

d er Rheolog
Pow y

ce Spec
p edan tro
-Im sc
o op
e y
Rh

Slurry Rheology Resource

Application Note:
Rheological Evaluation of Battery Slurries with Different Graphite Particle
Size and Shape

Shear and Flow Properties of an NMC Based Dry Cathode Powder

Characterization of LIB Cathode Slurries Using Simultaneous

Measurements of Rheology and Impedance Spectroscopy

eBook: Essential Battery Slurry Characterization Techniques

7
 Binder and Additive
In addition to ensuring proper electrode coating, the binder and additive in electrode slurries greatly contribute to the overall
performance. Binders require high thermal stability, good adhesion, and flexibility to facilitate proper battery performance. Low
quality binders and additives can cause cracking and chipping on the electrode coating.

Battery developers typically test binder and additive at two key stages:
• To verify incoming materials’ quality
• To measure the binder and additive’s composition and electrode performance

Thermogravimetric Analysis (TGA) measures weight change (loss or gain) and the rate of
weight change as a function of temperature, time, and atmosphere. Loss of mass indicates
possible decomposition or vaporization, while a gain in mass indicates possible oxidation,
sorption or that the material is reacting with the purge gas.

In batteries, TGA quantifies the amount of binder and additive in the electrode. This
measurement helps ensure the same amount of active material, binder and additive are in
each batch of electrode. On the Discovery TGA, the high sensitivity Tru-Mass Balance is ideal
for binder and additive testing as it ensures accurate measurement of each component in
the electrode. Insufficient amounts of binder will affect the active the electrode material’s
adhesion to the metal collector; too much binder will reduce the active material’s content and affect the electrochemical
reaction. Optimization of binder/additive ratios is essential for optimal battery performance and improvement of battery life.

TGA also measures the thermal stability, degradation temperatures, and content and composition of binder and additive.
Thermal stability can help identify the right composition and types of the binder to ensure proper performance during
electrode manufacturing.

Differential Scanning Calorimetry (DSC) measures binder melting and crystallization as

well as glass transition. Crystallinity is related to a binder’s mechanical properties, so this
measurement can be used as a diagnostic to predict binder behavior. Glass transitions are
related to the binder’s flexibility, and DSC also reveals melting of the binder which will impact
the thermomechanical properties. Lithium-ion batteries typically operate at temperatures of
-20 °C to 60 °C. Higher temperatures can disrupt the solid-electrolyte interface (SEI), or even
lead to decomposition. Thermal analysis enables researchers to understand the thermal
stability of the electrode while optimizing slurry composition and solvent drying for improved
batteries.

© 2024 TA Instruments. A division of Waters Corporation. All rights reserved.

8
 Characterization for Binders and Additives

What to Measure Technique What it Means Why it Matters TA Instrument

• Thermal stability
Thermal stability of of binder
Decomposition temperature TGA Discovery TGA
the binders • Ensure incoming
materials quality

Composition of binder Ensure correct

Weight change TGA Discovery TGA
and additive composition

Brittle glassy state to a Impact on the binder

Glass transition DSC Discovery DSC
flexible rubbery state properties

• Ensure incoming
Phase transition on the
Melting and Crystallization DSC materials quality Discovery DSC
polymer properties
• Process optimization

Active Cathode and Anode Materials

A battery’s cathode, or positive electrode, is usually made of a metal oxide; the anode, or negative electrode is usually made
of graphite. The cathode and anode are capable of intercalating lithium ions during charge and discharge. The electrode
must hold lithium ions without changing its structure, offer good electrochemical stability with the electrolyte, and be a good
electrical conductor and diffuser of lithium ions. Additionally, the thermal stability and rate capability of the entire battery is
largely dependent on the cathode and anode material.

Battery researchers are investigating cathodes and anodes with higher specific capacities while maintaining structural,
chemical, and thermal stabilities along with low cost. Thermal analysis enables researchers and engineers to understand the
thermal stability (phase transition, melting, and decomposition) of electrode and binder materials for safer and longer lasting
batteries across all operational temperatures.

Dry Electrode Processing

Dry battery electrode processing is a growing technique that removes the toxic solvent and lowers the cost of electrode
manufacturing. Dry battery electrode processing can be improved with powder rheology coupled with temperature control.
Powder rheology measures the flowability, shear, compressibility, and wall friction of dry electrode mix to help optimize mixing
and processing conditions. Plus, new temperature control features for powder rheology on the Discovery Hybrid Rheometer
allow users to obtain crucial powder insights under application-specific conditions.

Cathode and Anode Resources

Application Note: Safety Evaluation of Lithium-ion Battery Cathode and Anode Materials Using Differential Scanning

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Electrode Problem Solving

What it
Challenge Solution Technique TA Instrument
Measures
Measure incoming powder
Inhomogeneous and Power flowability, Discovery HR with
batches for critical parameters
aggregated slurry caused Powder rheology cohesion and yield Powder Rheology
like powder cohesion and yield
by low quality powders strength Accessory
strength

Measure viscosity at different

Non-uniform and defects Shear viscosity, slurry
shear rates to optimize the Rheology Discovery HR
on electrode network structure
coating process

Coating levels or drip as Understand structural

Thixotropy and
a result of slurry deformation, rate of structural Rheology Discovery HR
structure recovery
formulation properties recovery during coating process

Delamination or electrode
Quantify binder content in final Binder and additive
chipping from poor TGA Discovery TGA
electrode to verify specifications composition
adhesion

Gain insights on quality Melting and glass

Low quality of binder DSC Discovery DSC
and grade of binders transition temperature

Dry battery electrode Use powder rheology with Discovery HR with

Power cohesion and
processing needs to temperature control to evaluate Powder rheology Powder Rheology
processing condition
be optimized dry mix properties Accessory

Discovery HR
Poor Conductivity in Characterize conductive Impedance under
Rheo-Impedance Rheo-Impedance
Electrode material network in slurry process conditions
Spectroscopy

Simultaneous electrical
Predict electrode Conductive network Discovery HR
impedance and rheological
conductivity from slurry Rheo-Impedance structure under Rheo-Impedance
measurements to gain insight in
coating processing conditions Spectroscopy
slurry conductive network

© 2024 TA Instruments. A division of Waters Corporation. All rights reserved.

10
 Separators
Battery separators are porous membranes that separate the anode and cathode while allowing transport of ions during
charge and discharge. Battery separators play a critical role in lithium-ion battery performance, including the prevention of
thermal runaway. Some of the requirements for a battery separator include:

• Good electronic insulator

• Minimal electrolyte resistance
• Mechanical and dimensional stability
• Chemical resistance to the electrolyte
• Prevent contact between the electrodes
• Readily wetted by electrolyte
• Uniformity in thickness and properties

A number of analysis techniques are useful for determining separators’ quality, stability, and integrity.

Separator Problem Solving

Challenge Solution Technique What it Measures TA Instrument

Thermal stability,
TGA decomposition, polymer Discovery TGA
Thermal assessments and inorganic content
Selecting high quality and
to understand
performing materials
material parameters
Melting temperature,
DSC Discovery DSC
crystallinity

Understand melt
Dimensional change
integrity, rupture
Separator shrinkage and loss as a function of
temperature, and TMA Discovery TMA
integrity at high temperature temperature, shrinkage
orientation effects to
and rupture temperature
aid material selection

Understand tensile
strength, tensile strain,
Temperature dependent
Prevent deformation during and rupture point
DMA mechanical response, Discovery DMA
manufacturing under tension to identify material
modulus and strength
capabilities and
limitation

Thermal analysis of separators includes TGA, DSC, and TMA. 120 10

Coated
Deriv. Weight d(Weight) / d(T) (%/ºC)

Weight Percent Loss: 37.16% Uncoated

100 8
Thermogravimetric Analysis (TGA) measures weight change Weight Percent Loss: 99.93%

and the rate of weight change as a function of temperature, 80

6
Weight (%)

Weight Percent Loss: 5.84%

time, and atmosphere. In separators, TGA helps researchers 60 465.1 ºC
4
determine the decomposition temperatures of separators. 40
Residue Percent: 55.06%

That data can then help them determine the composition or 465.1 ºC
2
495.5 ºC
20
percentage of individual compounds in the separator, a key 0

step for quality control. 0

0 200 400 600 800 1000
Temperature T (ºC)

TGA curves of coated separator (blue)

and uncoated separator (green)

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Thermogravimetric data is critical to setting proper temperature limits for Differential Scanning Calorimetry method
development. Differential Scanning Calorimetry (DSC) measures temperatures and heat flows associated with thermal
transitions in a material. DSC helps battery separator researchers analyze the melting temperature, impact on melting, and
further understand properties of the polymer content determined from the TGA results. DSC data is crucial in predicting how
different materials will impact the separators’ final properties.

Thermomechanical Analysis (TMA) measures changes in the dimensions of a sample as a

function of time, temperature, and force in a controlled atmosphere. TMA measures battery
separators’ shrinkage onset and rupture temperature. This data helps researchers confidently
characterize separators and investigate the potential impact of added coating formulations.
High reproducibility in TMA is especially important when measuring safety critical properties
such a melt integrity, as a ruptured separator can lead to internal short circuit in a battery that
may lead to thermal runaway.

When thermal analysis is combined with mechanical testing, it’s possible to understand
dimensional stability of a polymer’s length and shape, e.g., the polymer separator. This thermal and dimensional insight can
help prevent separator failure and ensure battery safety.

For mechanical analysis of separators, researchers use Dynamic Mechanical Analysis (DMA) which
measures the mechanical properties of materials as a function of time, temperature, and frequency.
One particular challenge is preventing undesired elongation of separator material, which leads to
deformation. DMA helps researchers understand tensile strength, tensile strain, and rupture point
to identify material capabilities and limitation. This data empowers labs to optimize separators for
specific applications, choosing adequate materials to offer the desired thermal and mechanical
stability at end-use conditions.

Storage modulus, loss modulus, and tan delta curves for uncoated and coated separators

Example Experiments
See how TGA, DSC, TMA, and DMA contribute to efficient and effective separator characterization in these application notes
with real experimental data:

Thermal Analysis of Battery Separator Film

Battery Separator Film Development: Impact of Coating

© 2024 TA Instruments. A division of Waters Corporation. All rights reserved.

12
 Electrolytes
One of the most critical battery components is the electrolyte, which transports
Lithium ions between the cathode and anode during the charge and discharge
process. Lithium-ion battery electrolytes are traditionally made of highly
flammable solvent with highly reactive lithium salts.

Gel polymer electrolytes are a new formulation of interest as they offer

strong electrochemical properties and improved safety over traditional
solvent-based electrolytes. Despite these advantages, gel polymer
electrolytes still require significant improvements to fully contend with
liquid electrolytes.

When electrolytes reach their thermal degradation temperature, they will

degrade and generate a highly exothermic reaction. When this reaction
happens inside a battery pack, the highly exothermic degradation leads to
thermal runaway if the heat is not removed from the battery.

How can you maintain battery temperature to avoid electrolyte

degradation and optimize electrolytes for improved battery safety?
Electrolyte thermal stability can be investigated with Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry
(DSC). Diagnostic thermal stability testing saves time and resources as the safest, most stable electrolytes can be selected
early in development.

TGA elucidates the decomposition temperature and solvent loss profile of electrolytes at high temperatures. This data
contributes to understanding the overall thermal stability of the electrolyte. Additionally, DSC measurements identify the onset
temperature and heat of reaction during exothermic decomposition. The heat of reaction can be used to estimate the heat
released during the battery runaway. Combining TGA and DSC helps researchers evaluate the safety hazards of their batteries
under chemical abuse and design effective thermal management systems.

How can you optimize the gel polymer electrolyte’s mechanical properties?
Gel polymer electrolytes uniquely act as both the electrolyte and the separator, so the mechanical concerns of a separator’s
ability to separate the electrodes also apply to this electrolyte formulation. Dynamic Mechanical Analysis (DMA) measures
the electrolyte’s temperature-dependent mechanical response, offering key insights into the electrolyte’s tensile strength,
tensile strain, and rupture point under specific conditions. DMA helps battery scientists identify their electrolyte’s material
capabilities and limitations, facilitating stages of electrolyte development through to QA/QC of electrolyte formulation. Gel
polymer electrolytes are a new formulation of interest as they offer strong electrochemical properties and improved safety over
traditional solvent-based electrolytes. Despite these advantages, gel polymer electrolytes still require significant improvements
to fully contend with liquid electrolytes.

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How can you facilitate efficient electrolyte manufacturing with effective formulations?
A key area of electrolyte research involves optimizing formulations for ideal pumpability during manufacturing. This step offers
ample opportunity for reduced cost and increased efficiency. Rheology enables engineers to measure viscosity and produce
electrolyte solvents with optimal pumpability during manufacturing.

Components in lithium-ion batteries, such as electrolytes, lithiated materials and solid-electrolytes interface on electrode, are
highly sensitive and reactive materials with atmosphere. Testing and handling of such materials must be done in an inert
environment. It can be challenging but necessary to analysis those samples under an inert testing environment to prevent
sample integrity is compromised by a brief exposure to nitrogen, oxygen, or water.

TA Instrument Discovery TGA and Discovery Hybrid Rheometers enable glovebox operation for Argon and Nitrogen environments,
providing reliable material data of atmosphere-sensitive samples.

Resources
Application Note: Thermogravimetry of Air Sensitive Materials - TA Instruments

© 2024 TA Instruments. A division of Waters Corporation. All rights reserved.

14
 Module Pack Materials
Thermal Management System
Battery thermal management systems (TMS) offer the opportunity to improve battery life and reduce overall battery cost –
however, they must be carefully designed for this purpose. Maintaining temperature uniformity within a cell, and from cell to
cell, requires proper understanding of the thermal conductivity and cooling capacity of the materials used in the TMS.

Optimizing thermal management systems with DSC, thermal conductivity meter and laser flash will reduce the overall cost of
the battery pack, plus ensure battery safety and efficiency.

Thermal Interface Materials

Thermal adhesive and phase change materials (PCM) are used to regulate the battery pack temperature.The heat produced
by the battery during use poses a threat of inducing thermal events and is detrimental to the performance of the battery
itself. The advantage of PCM is they can maintain stable temperature when materials undergo phase changes. Differential
Scanning Calorimetry (DSC) is especially helpful in optimizing PCM through measuring phase transitions, heat of fusion,
and heat capacity to evaluate the materials cooling capacity.

Thermally conductive adhesive successfully holds the battery in place despite heat and offsets heat that could otherwise
impede performance. Laser Flash and thermal conductivity meter are used to measure thermal diffusivity and thermal
conductivity. This data helps battery developers select the best materials to dissipate heat.

Successful thermal interface materials must offer excellent thermal conductivity and thermal stability. All of these parameters
can be evaluated using material analysis techniques.

Thermal Interface Material Problem Solving

Challenge Solution Technique What it Measures TA Instrument

Evaluate ability Thermal conductivity,

Identify impact on thermal Thermal Conductivity meter, Thermal Conductivity &
and rate to diffusivity, heat capacity,
management system Flash Diffusivity Analyzers
diffuse heat thermal resistance

Measure
Evaluating an adhesive’s Thermogravimetric Analysis Degradation, thermal
degradation Discovery TGA
operating temperature limit (TGA) stability
point

Understand
Design and optimize polymer Curing, glass transition
Differential Scanning
materials and processing structure temperature, heat Discovery DSC
Calorimetry (DSC)
conditions and thermal capacity
properties

Understand flow
Optimize application
and reaction Rheology Curing, viscoelasticity Discovery HR
conditions
time

15
Casing and Enclosure
The battery, which commonly weighs 300 kilograms (661 pounds), is mounted to the casing or enclosure. Battery casings are
integral for overall battery performance, as they protect all internal components against contamination, adverse atmospheric
changes, and damage from impact. Casings are commonly made of steel, aluminum or polymers composite. Battery casings
must be molded or formed into their required shapes while providing protection for the inner components, which can be
achieved through detailed material analysis and testing.

Casing and Enclosure Problem Solving

Challenge Solution Technique What it Measures TA Instrument

Understand Discovery DMA

material Mechanical property,
Predict lifetime and Dynamic Mechanical
mechanical modulus, creep and ElectroForce
performance under load Analysis (DMA)
properties and fatigue Mechanical Test
durability Instruments

Identify
dimensional Thermal expansion
Part delamination or failure Thermomechanical Analysis
changes that or shrinkage, thermal Discovery TMA
due to thermal change (TMA)
occur with expansion coefficient
temperature

Case degrade or Evaluate Degradation

Thermogravimetric Analysis
decompose during thermal thermal temperature, evolved Discovery TGA
(TGA)
events stability gas analysis

© 2024 TA Instruments. A division of Waters Corporation. All rights reserved.

16
 Technique Cheat Sheet
Thermogravimetric Analysis (TGA) measures weight change Rheology is the study of flow and deformation of materials
(loss or gain) and the rate of weight change as a function of under the influence of an external force or stress. In batteries,
temperature, time, and atmosphere. Thermogravimetric data rheology measurements are used to ensure successful
is critical to setting proper temperature limits for Differential material processing, optimize product performance, gain
Scanning Calorimetry method development. Other common insights into complex microstructures and develop novel
usages include measuring: materials. While viscometers are limited to measuring
viscoelasticity, rheometers provide more comprehensive
• Thermal and oxidative stability of materials
information for battery development, including:
• Moisture and volatile contents
• Composition of multi-component materials
Non-Newtonian Behaviors
• Decomposition kinetics and estimated lifetime of a product
• Shear thinning
• Effects of reactive or corrosive atmospheres
• Thixotropy
• Yield stress
Differential Scanning Calorimetry (DSC) measures
temperatures and heat flows associated with thermal
Viscoelasticity
transitions in a material. Common usage includes
• Storage Modulus
investigation, selection, comparison, and end-use
• Loss Modulus
performance evaluation of materials in research, quality
• Tan Delta
control and production applications. Properties measured
by TA Instruments’ DSC techniques include:
Rheology is especially crucial in forming battery slurries that
• Phase changes
form uniform, defect-free coatings required for production of
• Glass transition point
consistent, high-quality electrodes with high batch-to-batch
• Melting and crystallization
repeatability and low scrap rates. Additionally, rheology is
• Heat of reaction (enthalpy)
used to optimize the manufacturing and performance of gel
• Product stability
polymer electrolytes and adhesives.
• Reaction kinetics
Isothermal Microcalorimetry (IMC) is a non-specific and
Dynamic Mechanical Analysis (DMA) measures the
non-destructive technique for measuring the smallest
mechanical properties of materials as a function of time,
reactions in a material during a physicochemical process.
temperature, and frequency. In addition to quantifying
This is done by measuring the heat flow from the sample at
viscoelastic properties of materials, DMA can also quantify
a constant temperature. Isothermal microcalorimetry offers
finished component and product characteristics, reflecting
key battery insights:
the important contribution that processing has on end-use
• Heat management
product performance. DMA is commonly used to measure:
• Entropy changes
• Mechanical properties
• SEI formation
• Modulus and stiffness
• Full cycle parasitics
• Creep and stress relaxation
• Narrow cycle parasitics
• Glass transition temperatures (Tg)
and secondary transitions For whole battery testing, the Battery Cycler Microcalorimeter
• Cure and processing optimization Solution is able to measure heat flows during battery cycling
• Filler effects in composites on a fully integrated, flexible system. Data from the TAM IV
Isothermal Microcalorimeter data are both collected
and analyzed in one user interface, making it easy to
run experiments and analyze results. The Battery Cycler
Microcalorimeter Solution is revolutionizing whole cell testing
with the highest throughput, fastest data aggregation, and
best experimental efficiency of any testing solution available.

17
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