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L027919EN iBR Reliable Li-Ion Battery Solutions v8

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0% found this document useful (0 votes)
35 views40 pages

L027919EN iBR Reliable Li-Ion Battery Solutions v8

Uploaded by

jiawei wang
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd

Reliable Lithium-Ion Battery Solutions

Exploring Materials, Components, and Quality Control


Table of Contents

Introduction

1. Manufacturing Needs through the Battery Workflow

2. Testing through the Battery Value Chain

3. Recycling of Used Lithium-Ion Batteries – Recovering


Valuable Elements

4. Service and Software Offerings

5. Additional Information
Introduction

Efficient, safe, and rechargeable batteries are essential


to today’s economy, and the demand is relentless
with the global adoption of small portable electronics,
uninterruptible power supplies, and electric vehicles.

Manufacturers need reliable instrumentation to develop new


technologies and ensure the quality of their products across
the value chain. METTLER TOLEDO instrumentation and
software support scientists through R&D, performance testing,
quality control, manufacturing, and recycling of batteries.

This guide explores materials and components along the


battery value chain and presents a comprehensive view of
the manufacturing and testing requirements to examine every
facet of lithium-ion batteries. Discover how you can leverage
precision technology to optimize every step of your workflow.
Manufacturing Needs through the Battery Workflow
Lithium-Ion Battery Production

A lithium-ion battery runs through up to 25 production steps,


from initial raw materials to a high-quality end product. The
most crucial ones lay the foundation for the highest battery
performance. A balance must be found between maintaining
high throughput and maximizing production yield.

Visit our Lithium-ion battery page


The Battery Manufacturing Workflow

Upstream Midstream​ Downstream​ End-of-Life (EoL)

Raw Materials ​ Raw Materials Battery Components Cell ​ Mechanical Reuse and Recycle
Preparation​ Processing​ Production​ Production​ Assembly​

Mining of Production and Electrode produc- Cell Module Second life as


mineral salts QC of battery tion and QC assembly​ production​ energy storage
grade and active (refiling)​
Refining of mined materials Separator QC​ Electrolyte Pack
materials preparation production Recycling to
and QC​ reclaim all
minerals and
Electrolyte filing​ metals​

Cell finishing
and QC​

Precision measurements in Controlled oxygen Accurate weighing in hazar- High precision weighing Weight-based QC Raw material recovery
Quality Determinants

harsh environments dous conditions


Controlled pH low oxygen Low water
Metal ions purity Monitor particle size Low water
HF content
Moisture analysis Metal ions purity Thermal stability of materials
Degradation, impurity and
Known metal purity polymerization
Defined porosity
Thermal stability and
behavior

*Click on each quality determinant to find tailored solutions for optimization.


Mining and Refining of Raw Materials

Mining operations place serious demands on their equipment.


Challenging environments and around-the-clock operations
require tools that are purpose-built to withstand tough
conditions and deliver reliable results.

METTLER TOLEDO provides you with a broad portfolio of


vehicle scales, balances, quality control analytical
instruments, and process analytics sensors that offer
critical durability under high temperature and pressure.​

Download our brochures covering weighing,


process analytics and quality control in the
mining process.
Ensuring High Quality PCAM Materials for NCM Cathodes

For NCM-type cathodes, PCAM is made through Particle size and shape are critical
the co-precipitation of nickel, cobalt, and pieces of information during co-
manganese hydroxides under tight pH control precipitation. Particle properties and
and inert atmosphere.​ particle mechanisms are recorded for
review and analysis.

Apart from stirrer speed and ammonia Purging the reactor with nitrogen
concentration, pH is a critical process eliminates oxygen, which otherwise
variable that determines particle morphology would lead to the undesired formation
and size. Depending on the required particle of metal oxide contaminants.
size distribution, process pH typically lies
between pH 9.0 and pH 12.0
Ensuring High Quality Calcination Process for CAM Production

CAM is made through the reaction of PCAM


and lithium hydroxide (or lithium carbonate),
and some dopants in a rotary calciner. During
O2 Exhaust Gas

the reaction, two solids react to form a new Purge Gas


compound, and gases are released in the
process. Depending on the CAM composition,
the atmosphere in the calciner can range Feed

from air to pure oxygen. Calciner oxygen


Air/Oxygen
concentration should, therefore, be precisely
controlled.

Fuel Gas

CAM Product

Download our application note to learn more


about CAM crystal structure
METTLER TOLEDO Offerings for
High-Quality PCAM Materials

METTLER TOLEDO offers unmatched solutions for monitoring


pH, oxygen, and particle characterization to ensure the highest
grade of Cathode Active Materials (CAMs).

Watch our webinar on​PCAM


production for lithium-ion batteries

Download our application note on


lithium-ion Battery Manufacturing
Slurry Blending and Formulation

Slurry blending occurs in hazardous environments, where


electrode materials are dispersed in an organic solvent and
stored in tanks. The amount of material weighed to create
the slurry is critical, and inaccuracy directly impacts battery
quality and safety in the production area.​

High-accuracy weighing is required to avoid material waste


and ensure battery quality.

Download our application note on​Weighing


in Hazardous Areas
Electrolyte Filling

After electrode stacking, the battery cells are filled with the electrolyte. High-precision weighing
is the ideal solution to control electrolyte flow, ensure quality, and avoid damage due to battery instability.
METTLER TOLEDO offers two different strategies for electrolyte filling.​

Precision Sensor Precision Sensor

Option 1 Option 2
The sensors ensure correct filling by providing feedback to the filling device. Weight-based filling ensures the highest precision, constant filler adjustment,
This solution offers flexibility in cell designs, no contact with the electrolyte, self-control, and adjustment for consistent cell quality.
and certifies consistent cell quality.​
Perfecting Lithium-Ion Battery Finish

The process of combining battery cells into modules and


then modules into complete battery packs involves welding,
bonding, and testing. This process requires high-resolution
scales for weight-based quality control of the cell/module
bonding and final battery pack.

Download our e-book on lithium-ion


battery production
Accurate Weighing in Battery
Production

The high-quality standards in battery production require


expertise in high-precision weighing. METTLER TOLEDO offers
a variety of solutions to achieve accurate weighing. These
technologies enable consistency and traceability in raw
material blending, inventory control, slurry mixing, electrolyte
filling, and in-line quality checks.

Watch our webinar on weighing strategies


to improve quality in battery production
Testing through the Battery Value Chain
The Main Battery Components Will
Affect Battery Performance and Safety

Procuring necessary raw materials and preventing battery


failure is imperative for lithium-ion batteries to dominate the
alternative energy revolution. Investing in the proper analytical
instruments to assess the integrity of different components
(separators, binders, electrolytes, and electrodes) will ensure
battery safety and reduce the risk of failure.
Sample Preparation

Accurate weighing is key in battery research and characterization labs


making efforts towards safe, high-performance, and affordable batteries.

Weighing applications include: METTLER TOLEDO laboratory balances and


• Weighing in sample and standard accessories –​​ such as antistatic solutions –
preparation for characterization: help simplify the difficult process of battery
- Electrolyte testing, e.g. by research, development, and characterization.
Karl Fischer titration
- Metal and purity characterization,
e.g. by ICP-OES
- Chromatography (e.g. HPLC, GC, IC)
- Thermal analysis (e.g. DSC, TGA)
- Spectroscopy (e.g. UV/Vis)
• Electrode slurry formulation
Moisture and Water Determination

To minimize electrode damage, and battery The Moisture Analyzer HX204 rapidly achieves
capacity reduction, water must be controlled highly repeatable results that correspond to
during the entire manufacturing process, from the drying oven reference method when used
goods-in to final product. Loss-on-drying to measure moisture in the electrode slurry. ​
methods are ideal for measuring moisture
content for goods-in and in-process quality METTLER TOLEDO Thermogravimetric Analyzer
control. (TGA) and balances (for drying oven method)
can also be used for such an application.

Read our application note on using a Download our guide on moisture and
Moisture Analyzer to measure moisture water determination
in a lithium-ion battery​
Karl Fischer titration is a precise technique The water content in the electrolyte is
that is used to measure trace water content generally measured before it is filled into
in battery materials. ​ the battery.​

For low water concentrations (ppm), the METTLER TOLEDO method M882 was
Coulometric Karl Fischer titration is the developed to accurately measure electrolyte
preferred method, and scientists often use it water content using HydranalTM NEXTGEN
with an external sample oven to analyze solid Coulomat reagents A-FA/C-FA, using a
materials. Coulometric KF Titrator C30S.

Read our application note on using Learn more about H2O and HF
Karl Fischer Titration to determine water determination in lithium-ion Batteries
content in electrode materials.
Titration Applications

Metal Ions Purity Determination and Determination of Iodine Adsorption


Impurity Detection Number of Carbon Black
Titration is commonly used in several norms The surface porosity of the carbon black
and standards to determine the purity of is commonly measured using the iodine
the metal content (cobalt, manganese, iron, adsorption number.
nickel) or assess the presence of impurities
(chlorides, lithium hydroxides, and lithium METTLER TOLEDO method M798 was
carbonate) in the electrodes. developed to help you measure the iodine
adsorption number according to ASTM
D 1510-16 standard, using our Titration
Excellence instruments.

Read our application note on Metal Download the method and the related
Titration Applications application note on iodine adsorption
number here.
Determination of Hydrofluoric Acid METTLER TOLEDO’s method M813 for HF
(HF) Content ​ determination is based on acid-base titration
HF is detrimental to the battery. Acid-base and achieves a good repeatability with
titration has proven to be an accurate and a standard deviation of 1.7%.​
reliable method to test the presence of HF in
the electrolyte solution.​

METTLER TOLEDO Titrators are recommended


for these applications, while Analytical
balances and pipettes are ideal for sample
preparation.​

Read the full application note: HF Content of


lithium-ion Battery Electrolyte
Assessing Material Behavior and Safety

For R&D or quality control, assessing material stability, understanding


chemical composition, and thermal behavior is important for predicting
performance under harsh conditions.

Thermal analysis techniques such as TGA and Calorimetric measurements using the RC1
DSC provide precise measurements for heat automated reactor will complete the risk
capacity, decomposition temperatures, and assessment on battery stability and provide
enthalpy determination to assess the thermal information on performance and safety.​
stability and safety of each component
developed and used in batteries. With these
tests, the optimal operating temperature range
of the battery can be determined, and steps
can be taken to avoid thermal runaway of
batteries.

Download our guide on thermal analysis for


battery research and QC
Softening Point of Pitch

Petroleum pitches are applied to the surface of graphite


to improve the electrochemical properties of electrodes.
Measuring the softening point of the pitches is critical when
assessing their suitability and ensuring optimal electrode
performance.

Read our application note on


Softening Point of Pitch
Physicochemical Characteristics of
the Liquid Electrolyte and Solvents

Impurity Analysis Degradation Analysis ​


UV/Vis spectrophotometry is used to analyze To identify changes in the chemical
the electrolyte solution and detect the composition of the electrolyte, scientists
presence of impurities by comparing the compare the absorption spectra of the
sample absorbance/transmittance color electrolyte to a baseline spectrum. Changes
number with a reference color scale, e.g., provide insight into the degradation
APHA, CIELAB, or Hazen. mechanisms of the battery.

Watch our Video on how to measure the


color of an electrolyte​
Polymerization Monitoring Measurements of pH, conductivity, density,
Inline and offline pH and conductivity refractive index, and UV/VIS color are used to
measurements of the electrolyte solution evaluate the lithium-electrolyte and solvent
enable the detection of the polymerization of quality. These physicochemical characteristics
electrolyte materials. can be measured using analytical tools from
METTLER TOLEDO.

Read our application note on Read our application note on


Fully Automated Multiparameter Analysis Conductivity of lithium-ion Battery
of lithium-ion Electrolyte Electrolyte
Recycling of Used Lithium-Ion Batteries – Recovering Valuable Elements
Repurposing Lithium-Ion Batteries

With the growth in applications involving lithium-ion batteries as energy 400 kg


storage, the increasing demand for raw materials is bound to harm the
environment and the planet’s resources.

Capacity 50kWh
Repurposing and recycling the spent batteries Recycling efforts mainly focus on recovering
and batteries that did not meet quality metals such as aluminum, nickel, cobalt, iron,
requirements is becoming a strategy to copper, calcium, manganese, and lithium.
reduce the burden of toxic waste and pollution Researchers are also defining processes to
associated with lithium-ion battery disposal. recycle graphite, electrolyte components, and
separator materials.
Aluminium, 126kg Manganese, 12kg
Graphite, 71kg Cobalt, 9kg
Nickel, 41kg Electronics, 9kg
Electrolytes, 37kg Lithium, 8kg
Copper, 22kg Steel, 3kg
Plastic, 21kg Others, 41kg
Enabling the Efficient Recovery of Valuable Materials

With battery recycling, companies are creating a circular economy to reclaim, recycle and reuse critical materials.
The following steps are being used in the process of recycling lithium-ion batteries.

1 2 3 4 5

Characterization Dismantling, deactivating, Removal of volatile Recovery of metals Quality control and
of the type of battery and shredding electrolyte residues like cobalt and lithium characterization
being recycled, including the battery cell under inert through pH dependent of recycled materials
chemical composition, atmospheric conditions to precipitation of salts. using elemental analysis
size, shape, and state of avoid thermal runaway. to ensure they meet the
charge. required specifications.
Battery Recycling Applications Dismantling and Shredding
• Weighing

Electrolyte Recovery
• Karl Fischer water measurement
Recycling applications are similar to upstream • HF Titration
applications. METTLER TOLEDO’s innovative • Conductivity
solutions support various steps in the battery • Thermal Analysis
LiPF6 Organic • Lithium Titration
recycling value chain, from pH and ORP • Weighing
Carbonates
monitoring while recovering raw materials
and separating components to final quality
control.​ Anode, Cathode, and Metal Separation
• pH of carbon black
• ISE for ion content
Fe, Al, Cu, Graphite • Karl Fischer or Moisture Analyzer for
water and solid content
• Thermal Analysis
• Metal Titration
• Weighing

Cathode Leaching and pH Precipitation


Material
Cathode Material • Inline pH and ORP
• Metal Titration
• Weighing

Find out more about our process analytics


application for battery recycling
Service and Software Offerings
Productivity through Software

Automation ​ Complete Data Collection​ Support from METTLER TOLEDO Software​

Automation not only improves the reproducibility Automatic and real-time capture of complete METTLER TOLEDO software maintains protocols,
of experiments and increases user safety, it data sets, with central data management and drives measurements, analyzes data sets, and
also enables data continuity while maintaining customizable reports, prevents time-consuming securely stores results in a database or LIMS.
accuracy. ​ rework and increases efficiency, traceability, Moreover, the software offering provides structure
and data quality​ and a paperless data trail for accurate audits.​

www.mt.com/lab-automation www.mt.com/data-integrity www.mt.com/Lab-software


www.mt.com/ind-automation-components www.mt.com/ind-software​
Efficiency through Service

Service of the Instruments ​ Cleaning and Appropriate Use of the Instrument Calibration of the Instruments​

Equipment often accounts for a large portion of To ensure optimal equipment performance, the Regular calibration is critical in ensuring the
overall expenses. To ensure optimal instrument operators should be knowledgeable and well- accuracy, repeatability, and standardization
performance over time, keep repair costs down, trained in equipment use and maintenance. of the scales and sensors of your analytical
and reduce instrument and parts turnover, Cleaning is an essential step after instrument use; instruments.
performing regular preventive maintenance on the it will prevent or lower the risk of contamination
equipment is indispensable. and damage.

www.mt.com/service www.mt.com/ind-rapidcal
www.mt.com/ism-sensors​
METTLER TOLEDO Good Measuring Practices

With METTLER TOLEDO’S Good Measuring


Practices, we help you improve your
measuring process with a standardized
approach developed for the proper selection,
calibration, and routine operation of your
instrument. Good Measuring Practices cover
your equipment’s entire life cycle and help you
improve quality while reducing risks and costs.

www.mt.com/gp-collection
Additional Information
Product Offering

Laboratory Weighing Industrial Weighing


Electrodes Sample preparation Analytical balances Formulation (Hazardous Solution) PBK989/PFK989 IND500x Form+
Dry content of electrode slurry Halogen Moisture Analyzers Mixing process (Hazardous Solution) SWB605, SWC615-A, IND570, IND360, ACT350
Bulk and simple weighing PFD779, IND570, IND331, SWB505, SWC515-A, PBA430,
ACT350
Electrolyte Sample preparation Analytical balances Electrolyte filling WMF, WMS
Filling and mobile weighing (Hazardous Solution) PFD779, IND570, PUA579, IND256
Formulation (Hazardous Solution) PBK989/PFK989, IND500x, Form+, SWB605, SWC615-A,
IND 570, IND360, ACT350
Bulk and simple weighing PFD779, IND570, IND331, SWB505, SWC515-A PBA430,
ACT350
Separator Sample preparation Analytical balances
Raw material moisture content Halogen Moisture Analyzers
Mining, Raw Vehicle weighing Truck Scales / Weighbridges, Rail Scales, POWERCELL®
Material Processing, Smart Load Cells, IND9U, Unattended Terminal,
Material Transport DataBridge™ Transaction, Management Software

www.mt.com/labweighing
www.mt.com/ind-solutions
Laboratory pH and Titration and Karl Fischer UV-Vis, Density and Dropping Point Material Characterization
Conductivity
Electrodes pH, conductivity S475 Meter Water content C30S Compact Titrator with InMotion Metal ions (e.g., Al, As, Fe, UV5, Cuvette Changer Phase transition point of the DSC,
values Karl Fischer Oven Autosampler Si, SiO42-, Co, Mn, Ni) InMotion UV/VIS, Easy UV cathode material, thermal stability TGA
ISE: F- ions PerfectION Metal content Potentiometric Titrator with InMotion Anode production DP 70/90 Determination of active material TGA
(Cathode) comb F (Li, Mn, Co, Al), acid Autosampler content
content, LiOH purity
Iodine absorption Titrator Excellence Density of slurries D4 Decomposition analysis TGA
(carbon black)
Conversion of graphene oxide into TGA
(Anode)
graphene (Anode)
Electrolyte pH, conductivity S475 Meter Water content Coulometric Karl Fischer Titration Metal ions (e.g., Al, As, Fe, UV5, Cuvette Changer Electrolyte analysis (type, DSC,
values Si, SiO42-, Co, Mn, Ni) with InMotion content, thermal stability, melting TGA
Autosampler behavior).
Color UV5, UV7, Easy UV Usable temperature range DSC
Density D4
Separator pH value (AI) S475 Meter Water content C30S Compact Titrator with InMotion QC of microporous separators DSC, TGA,
Karl Fischer Oven Autosampler – diaphragm analysis (type, TMA,
content, actual failure temperature) DMA

www.mt.com/phlab www.mt.com/uv-vis www.mt.com/thermal_excellence


www.mt.com/titration-pp www.mt.com/dropping-point www.mt.com/density
Automated Reactors and In-Situ Analyses Process Analytics
Electrodes Precursor cathode active material ParticleTrack, EasyViewer Precursor cathode active material - crystallization InPro 4260i, InPro 6850iG, InTrac 777 M400-2w,
crystallization EasyClean 200
SiOx synthesis ReactIR, ReactRaman Precursor cathode active material - filtration and washing “Unicond 4 Electrode”, InPro 3250i
Precursor cathode active material - cathode active material GPro 500 oxygen analyzer
calcination
Electrolyte IPC of electrolytes/aditives ReactIR, EasySampler, ParticleTrack,
LiPF6 crystallization EasyViewer
Calorific values and risk RC1mx, EasyMax
assessment

www.mt.com/autochem
www.mt.com/process_analytics
Additional Reading

PCAM and Cell Manufacturing Titration and Karl Fischer Titration

• PCAM Degradation • Determining Purity of Lithium Hydroxide Using the InMotion Autosampler
• 7 Steps to Select the Right Scale for Filling Machines • Water Content of Lithium-Ion Battery Electrolyte with KF Titration
• Checklist Provides Guidance for Integrating Automated Weighing into Machines • Coulometric KF Titration of LIB Electrolyte
• 7 Reasons to Use Automated Precision Weighing • Determine the Purity of Lithium Hydroxide by DispenSix Liquid Handler
• Lithium Carbonate and Lithium Hydroxide Content of Cathode Material

Density Measurements • Cobalt Content of Lithium Cobalt Oxide based Cathode Material

• Determine the Water Content of NMP by Density • Chloride Content of Lithium Cobalt Oxide based Cathode Material

• Lithium-Ion Battery Density • Total Iron Content of Lithium Iron Phosphate Battery based Cathode Material
• Manganese Content in NMC Cathode Material
• Cobalt and Nickel Content of Lithium-ion Battery NMC Cathode Material
UV-Vis Measurements
• Potentiometric Determination of Lithium-ions in Batteries
• Easy UV Vis Color Measurement of over 30 Color Scales
• Total Metal Content in NMC Cathode Material of Lithium-ion Battery
• Metal Content in NMC Cathode Material of Lithium-Ion Battery by Complexometric
pH Measurements Titration with a Cu-ISE
• Battery Analysis: pH of Cathode Material • Sodium Content in Battery Electrolyte Using Multiple Standard Addition
Sources

Baum, Zachary J., Robert E. Bird, Xiang Yu, and International Energy Agency “Global Supply Chains The Analytical Needs for Recycling Lithium-Ion Batteries.
Jia Ma. “Lithium-Ion Battery Recycling–Overview of of EV Batteries,” Accessed May 25, 2023.​ Nowak, Sascha. Lab Manager. July 19, 2021.​
Techniques and Trends.” ACS Energy Letters 7,
no. 2 (February 11, 2022): 712–19.​ Lu, Lei-Lei, et al. “Extremely Fast-Charging Lithium “The Crucial Race to Build a Better Battery: Big Brains
Ion Battery Enabled by Dual-Gradient Structure Design.” Podcast with Shirley Meng | University of Chicago News.”
Bergamin, Fabio. “Progress in Alternative Battery Science Advances, vol. 8, no. 17, 29 Apr. 2022. News. uchicago.edu, 4 Aug. 2022.
Technology,” April 24, 2023. Accessed 25 Sept. 2022.​
Volkswagen Group. “Battery Recycling Plant.” Accessed
Bergamin, Fabio, and E. T. H. Zurich. “New Zinc Metal MIT News | Massachusetts Institute of Technology. May 31, 2023.​
Batteries Can Be Cheap, Efficient, Durable, Safe and “A New Concept for Low-Cost Batteries,” August 24, 2022.​
Environmentally Friendly.” Accessed May 22, 2023.​ World Economic Forum. “‘Renewables’ Power Ahead to
MIT Technology Review. “What’s next for Batteries.” Become the World’s Cheapest Source of Energy in 2020.”
Campbell, Maeve. “Could Replacing Lithium with Salt Accessed May 22, 2023.​ Accessed September 30, 2022.​
Solve the Battery Crisis?” Euronews, 9 Feb. 2022.
Petrova, Magdalena. “Here’s Why Sodium-Ion Batteries Are Zhou, Li-Feng, Dongrun Yang, Tao Du, He Gong, and
Engel, Andreas. “Les voitures électriques sont-elles Shaping up to Be a Big Technology Breakthrough.” CNBC, Wen-Bin Luo. “The Current Process for the Recycling of Spent
réellement vertes?” Blick, May 30, 2023. May 10, 2023.​ Lithium Ion Batteries.” Frontiers in Chemistry 8 (2020).​

Feasibility of utilising second life EV batteries: Applications, ScienceDaily. “New Battery Technology Has Potential
lifespan, economics, environmental impact, assessment, to Significantly Reduce Energy Storage Costs: New, Low-
and challenges. (2021). Alexandria Engineering Journal, Cost Battery Built with Four Times the Capacity of Lithium.”
60(5), 4517–4536. Accessed May 22, 2023.​
www.mt.com METTLER TOLEDO Group Subject to technical changes.
Laboratory - Divisional Marketing © 10/2023 METTLER TOLEDO. All rights reserved.
Local contact: www.mt.com/contacts L027919EN
Group MarCom RITM1049959 NM/PH/BM

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