Understanding the Lithium Ion Battery from Surface to Cell

Understanding the Lithium Ion Battery from Surface to Cell

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Description: Detail the Li-ion Battery industry drivers & trends, Our position in the industry and our interest in the application, Battery research overview, How the LiB works and targeted research problems, Application capabilities, Example LiB solutions to tough problems, Sample Discussions/LiB Inquiries. Our Responsibility Behind Understanding LiB: We have the responsibility to add our experience in the areas of research that make our world healthier, cleaner, and safer. Build new Solutions that take a closer look at the materials, changes, and future of battery analysis.

Help our global partners achieve their long-term research goals!.

 
Author: Molly Isermann  | Visits: 405 | Page Views: 689
Domain:  Green Tech Category: Battery & Fuel Cell 
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Contents:
From Surface To Cell: Understanding
the Lithium Ion Battery
Molly Isermann
Vertical Marketing Manager
Market Development

Proprietary & Confidential

The world leader in serving science
1

Content Discharge
•Detail the Li-ion Battery industry
drivers & trends
•Our position in industry and our
interest in the application
•Battery research overview
•How the LiB works and targeted
research problems
•Application capabilities
•Example LiB solutions to tough
problems
•Sample Discussions/LiB Inquiries

2

Global Drivers
Global Market Objectives

Drivers
•Safety
•Consumers Needs
•Emissions control
•Globalization in Regulatory
•Funding, investments, infrastructure
•Growing performance needs

Result
•Reliable Sustainable energy
•Controllable technology
•Predictable energy storage and generation

•Reduce environmental hazard
•Reduce cost to manufacture
•Increase power & energy of LiB
•Breakdown monopoly
•Enhance warranties and consumer
confidence

Market Influence
•Pervasive technologies- Auto
•Plateau of available LiB power
•Limit to fuels and alternative energy
resources
•Start-ups, JVs, regional shifts

Forecast
•End market CAGR 23.3% 2013-2020
•By 2013 >100 competitive players in LiB
•EV market to be 2X consumer LiB by 2023
Strong funding of academic, contract labs,
and government funded test-houses

3

Our Responsibility Behind Understanding LiB
We have the responsibility to add
our experience in the areas of
research that make our world
healthier, cleaner, and safer.
.
Build new Solutions that take a
closer look at the materials,
changes, and future of battery
analysis.
Help our global partners achieve
their long term research goals!
4

The Ten Year Cycle of R&D to Market

Property of Argonne National Laboratory: https://anl.app.box.com/batterytechnologyreadiness

5

How the Lithium-ion Battery Works

Chemistry:
•LCO
Lithium Cobalt Oxide

•LFP
Lithium Iron
Phosphate

•LMO
Lithium Manganese
Oxide

•NMC
Nickel Manganese
Cobalt Oxide

•NCA
Ni Cobalt Al Oxide

•LTO
Lithium Titanate
6

Rechargeable
Deintercalation
Intercalation

LiB Value Chain
Raw
Materials

•Lithium
Compounds
•Electrolyte
organics
•Graphite
•Manganese
•Nickel
•Cobalt
•Copper
•Aluminum

7

Cell Components

•Anode
•Cathode
•Electrolyte
•Separator
• Binders
•Chemicals
•Carbon Materials

Systems

•Cells
•Packs
•Electrode
coating
•Cell Assembly
•Testing Houses

Accountable for almost half
of the costs in LIB!

End Market

•Proprietary
technology for
output and
operation
•Battery Pack
Design for host

Research Tradeoffs
Balance between tradeoffs is critical to successful research!
How do we maximize the balance?
SAFETY

LIFETIME

POWER/
SCALE

•Fires
•Environmental
Impact
•Temperature
Risks
•Consumer &
Laboratory
Safety
•New Materials
& Adverse Risks

8

CAPACITY
/ ENERGY
•Predictability
•Cycle Effects
•Reproducibility
•New Materials
•Physical &
Chemical
Impact
•Charge
Transfer

•Warranty
Enhancements
•Reliability of
Fuel Source
•Short
Prevention
•Chemical
Changes
•Physical
Problems

•Consumer
Electronics and
Automobile
•Scalable
Research
•Commercial
Transfer

Key Problem Areas- The Battery Breakdown

Cell

Separator

Binder

Anode

•In situ activity
•Optimum cell
chemistry
•Prevention of
leaks
•Internal
Impedance
•Stability of
varying
components and
cell
9

Electrolyte
•Additives
•Ion dispersion
•Gas generation
•Flammability
•Low flashpoint
•Breakdown
products

•Porosity effects
•Copolymer
characterization
•Resistance
•Mechanical
strength
•Impurities
•Thickness
•Temperature
Limits

•Homogeneity
•Surface area
control
•Composition
•Heat resistance
•Material
variance
•Impurities
•Viscosity
•Adhesion

•Lithium
deposition
•Dissolution
•Expansion
•SEI Layer
•Silicon Behavior
•Ion Dispersion
•Particle
Morphology

Cathode
•Oxide
formations
•Volume changes
•Film growth
•Functional
group ID
•Dendrites
•Impurities
•Capacity effects

How Might One Analyze the Battery?

Define Battery Question and Problems
Battery
disassembly
to analyze
Individual
Components
Upon
• Inert Sample change/failure.

ex situ

Transfer
• Reactive Analysis
• Destructive
analysis (Battery
De-assembled)
10

in situ

Analysis under
load, in a working
environment to
observe real-time
cell activity.

• Can view during
operation/charge cycles
• Put into a ‘real’ situation
• Assemble a battery
• Proactive Analysis

Key Problem Areas- in situ Cell Investigations

Cell

Electrolyte

Separator

Binder

Anode

•In situ activity
•Optimum cell
chemistry
•Prevention of
leaks
•Internal
Impedance
•Stability of
components and
cell

•Additives
•Ion dispersion
•Gas generation
•Flammability
•Low flashpoint
•Breakdown
products

•Porosity effects
•Copolymer
characterization
•Resistance
•Mechanical
strength
•Impurities
•Thickness
•Temperature
Limits

•Homogeneity
•Surface area
control
•Composition
•Heat resistance
•Material
variance
•Impurities
•Viscosity
•Adhesion

•Lithium
deposition
•Dissolution
•Expansion
•SEI Layer
•Silicon Behavior
•Ion Dispersion
•Particle
Morphology

11

Cathode
•Oxide
formations
•Volume changes
•Film growth
•Functional
group ID
•Dendrites
•Impurities
•Capacity effects

in situ Raman: Lithiation of Graphite

• Graphite coated on wire mesh current collector
• Representative area examined by Raman
12

Image and electrochemical data provided by
EL-CELL, use of ECC-Opto-Std optical
electrochemical cell, 2015

in situ Raman: Change in Spectrum Over Time
• Raman
band
shifts
10 cm-1
(1580
to
1590)

13

in situ Raman: Change in Raman Image Over Time

36
min

14

225
min

496
min

Key Problem Areas- Ex Situ Electrode Investigations

Cell

Electrolyte

Separator

Binder

Anode

•In situ activity
•Optimum cell
chemistry
•Prevention of
leaks
•Internal
Impedance
•Stability of
varying
components and
cell

•Additives
•Ion dispersion
•Gas generation
•Flammability
•Low flashpoint
•Breakdown
products

•Porosity effects
•Copolymer
characterization
•Resistance
•Mechanical
strength
•Impurities
•Thickness
•Temperature
Limits

•Homogeneity
•Surface area
control
•Composition
•Heat resistance
•Material
variance
•Impurities
•Viscosity
•Adhesion

•Lithium
deposition
•Dissolution
•Expansion
•SEI Layer
•Silicon Behavior
•Ion Dispersion
•Particle
Morphology

15

Cathode
•Oxide
formations
•Volume changes
•Film growth
•Functional
group ID
•Dendrites
•Impurities
•Capacity effects

Post Diagnostic Li-ion Battery Anode, 2yr Cycle

• Electrode material (dark areas) lies between overlayer of
separator particles (light areas)
• Red (29% area) & blue (20% area) are variations in SEI layer
• Green is separator particle
16

Ex situ Analysis of a Cross-Sectioned Anode Material
Cross-sectioned anode material in the ex situ transfer cell

The red color indicates the presence of carbon black while the blue color
represents graphite. The distribution of these materials on the two sides of
the electrode is significantly different. The copper current collector is in the
center.
50X long working distance objective, 532 nm laser (2.0 mW), area imaged 76 µm x 160 µm, image pixel size 1 µm,
0.2 s exposure time, 4 scans

17

Key Problem Areas- Surface analysis of Cathodes

Cell

Electrolyte

Separator

Binder

•In situ activity
•Optimum cell
chemistry
•Prevention of
leaks
•Internal
Impedance
•Stability of
components and
cell

•Additives
•Ion dispersion
•Gas generation
•Flammability
•Low flashpoint
•Breakdown
products

•Porosity effects
•Copolymer
characterization
•Resistance
•Mechanical
strength
•Impurities
•Thickness
•Temperature
Limits

•Homogeneity
•Surface area
control
•Composition
•Heat resistance
•Material
variance
•Impurities
•Viscosity
•Adhesion

18

Anode

Cathode

•Oxide formations
•Lithium
•Volume changes
deposition
•Film growth
•Dissolution
•Functional group
•Expansion
ID
•SEI Layer
•Dendrites
•Silicon Behavior
•Impurities
•Ion Dispersion
•Capacity
•Particle
effects
Morphology
•Lithium
Transfer

K-Alpha+ Sample Transfer Capability and weak signal
detection
Analysis Examples:
• Electrodes
• Surface characterization of pristine material

Inert atmosphere transfer
• Load samples in glove box
• Transfer under vacuum to K-Alpha+

• Confirm oxidation state, composition, Li
gradients
• Ex-situ characterisation after cycling
• Composition & variation with depth of SEI
• Variation in surface composition of electrode
material

• Separators
• Surface characterization of pristine material
• Confirm surface chemistry
• Ex-situ characterisation after cycling
• Look for polymer degradation
• Deposition of material from electrodes &
electrolyte

19

www.xps-simplified.com

XPS Comparison of Pristine and Cycled Cathode

Verification of Atomic %
Lithium loss from cathode
post-cycling

20

Key Problem Areas- Electrolytes

Cell

Electrolyte

Separator

Binder

Anode

•In situ activity
•Optimum cell
chemistry
•Prevention of
leaks
•Internal
Impedance
•Stability of
varying
components and
cell

•Additives
•Ion dispersion
•Gas generation
•Flammability
•Low flashpoint
•Breakdown
products
•Degradation
Products

•Porosity effects
•Copolymer
characterization
•Resistance
•Mechanical
strength
•Impurities
•Thickness
•Temperature
Limits

•Homogeneity
•Surface area
control
•Composition
•Heat resistance
•Material
variance
•Impurities
•Viscosity
•Adhesion

•Lithium
deposition
•Dissolution
•Expansion
•SEI Layer
•Silicon Behavior
•Ion Dispersion
•Particle
Morphology

21

Cathode
•Oxide
formations
•Volume changes
•Film growth
•Functional
group ID
•Dendrites
•Impurities
•Capacity effects

Example 1: Li-Ion Battery Analysis: IC-ICP-MS
IC-CD

IC-ICP-MS

Suppressed Conductivity Detection

iCAP Q ICP-MS

Bromide

100

Phosphate

Carbonate

Fluoride

Sulfate

μS

0.0
0.0

12.5

25.0

40.0

Time (min)

• Analyze 31P Containing Products in the Presence of Other Elements
22

Example 2: Li-ion Battery Analysis: IC-HRMS
IC-CD

IC-HRMS

Suppressed Conductivity Detection

Q Exactive Orbitrap MS
100

Phosphate esters

Step-wise Approach
3.78 min

2. Full scan MS/MS acquisition

3. Component ID based on HRAM
Data
4. Propose Structure

Exact
mass

Delta
ppm

C3H8O4P

139.0166

0.2

C2H6O4P

1. IC Separation using a KOH eluent
Relative Abundance

μS

Chemical
formula

125.0009

-0.1

m/z

• Component Identification in Untargeted and Unknown Workflows
Source for Dimethyl phosphate image: CSID:2982799, http://www.chemspider.com/Chemical-Structure.2982799.html (accessed 00:59, Feb 5, 2015)

23

Thermo Scientific Building Block of Application Solutions

Fourier
Transform
Infrared
Spectroscopy
(FTIR)

DXRxi Raman
Imaging
Microscope

•SEI formation
•Electrolyte
•Composition
degradation
changes
•Electrode volume
•Crystallization
and structure
•SEI growth
changes
•Dendrite formations
•Morphology of
•Functional Group ID
components
•Additive
•Homogeneity of
confirmation/ID
electrode
•Gas Emissions
•Composition
•Copolymer
changes
Characterization
•Ionic Dispersion
24

K-Alpha+: X-ray
Photoelectron
Spectrometer
(XPS)
•SEI growth
•Graphite
changes
•Porous Changes
•Electrode
structure
changes
•Dendrite
formation

UltraDry
Windowless
EDS Detector
•Oxide
formations
•Electrode
volume
changes
•Electrode
composition
•Electrolyte
solutions

ICP-OES,
ICP-MS, IC,
HPLC,
GCMS
•Impurities
•Electrolyte
solutions
•Emissions
Degradation
byproducts
•Metallic
dissolution

The Automotive and Advanced Materials Industry
Targeted Pieces
•Carbon Materials
•Glass technology
•Display Materials
•Lighting Advancements
•PowerTrain
•New Energy
•Renewable Energy
•Secondary Batteries
(Li-ion)
•Carbon Filled Materials
•Brake Advancements
•Lubricants
•Rubbers
•Adhesives
•Recyclables
•Plastics
•Paints & Coatings
•Laminates

25

Goals in Research
•Materials: Weight
•Reduction
•Materials: Strength
Enhancement
•Catalysis
•Scratch Resistance
•Safety
•Failure Analysis
•Fire Prevention (Flame
Retardants)
•Emissions Control
•Lifetime of Product
•Corrosion
•Resistance
•Corrosion Resistance
•Reduce, Reuse,
Recycle
•Heat Resistance
•Color Retention

2015 Activity and Tool Development
Materials Development
•Application Solutions
•Snapshots
•Webinar Series
•Educational Newsletter
•New Automotive
and New Energy Landing Page
•Interactive Video(s)
Building our Credibility
•Samples from collaborators
•Workshop(s) & Training
•Solution Developments
•Sample Inquiry Form (Sample Submissions)
26

Thank you!
For Additional Questions Contact:

Molly Isermann
Vertical Marketing Manager: Market
Development
608-276-5664
Molly.isermann@thermofisher.com

27