Complexity of Battery Grade C-LiFePO4 Development and

Complexity of Battery Grade C-LiFePO4
Development and Quality Management
Thorsten Lahrs
CEO, Phostech Lithium
THE 27 th INTERNATIONAL BATTERY SEMINAR & EXHIBIT
Primary & Secondary Batteries - Other Technologie
March 15 - 18, 2010
Broward County Convention Center
Fort Lauderdale, Florida

Pyrolytic Carbon Deposit (PCD)
Pyrolysis of most organic
materials during or after
LiFePO4 synthesis leaves a
conductive C deposit.
Organic precursor can be
solid, liquid or gas.
Carbon deposit is bonded on
elementary particles or on
agglomerates = C-LiFePO4
PCD controls sintering and helps
preserve Fe precursor or LiFePO4
size & shape, e.g. 50nm to 15µ.
LiFePO4
200 nm 100 nm
2 µ agglomerate
Carbon
deposit
Key to material power, optimal energy and cyclability

Phostech Production Processes
Process Solid State Wet Process Melt
Grade Energy Power Alternative
Status Commercial P1 Commercial P2
Pilot
Scale
Phostech Lithium controls several synthesis processes to
fulfill needs of present & future customers and markets

Phostech Commercial Products
P2 - Power Grade
P1 - Energy Grade
Nanosized Micro-Aggregates
+ Under-development products to fulfill customers needs
Strong R&D investment to continuously improved products

LiFePO4 Production Capabilities
500 tons/year
Life Power® P1 in Québec
250 tons/year
Life Power® P2 in Germany
Capacity expansion planned

LiFePO4 Market Main Advantages
Phostech Lithium introduced LiFePO4
on market with a specific brand name:
Life Power®
•Significantly more stable and therefore
safer than conventional cathode materials
•More cost-effective as no very rare and
expensive cobalt
•High-power & Fast-charge capabilities
•Wide temperature tolerance ensuring
performance at -40°C
Life Power® quality recognized by battery industry

Life Power® P1 Solid State Process
FePO4 + ½ Li2CO3 + C-precursor C-LiFePO4
+
-
•Simple: mixing + heating
•Low cost equipment (furnace)
•One-step reaction
•Depends on Fe 3+ ion-diffusion
•Depends on solid reactants mixing quality
•Non-reversible side reaction
•Cost of precursors (FePO4)
Energy grade C-LiFePO4
=> Improved power grade in development

+
-
Life Power® P2 Wet Process
Fe source + Li source + P source LiFePO4
LiFePO4 + C-precursor C-LiFePO4
•Low cost reactants
•Complete reaction in liquid phase
•Q/C & chemical purity control at each step
•Particle size, morphology and purity control by precipitation
•Consistency => low rejects and narrow cells specifications
•Nano-sized primary particles for power applications
•Capital intensive manufacturing process
•Require large scale installations
Power grade C-LiFePO4
=> Improved energy grade in development

Ragone plot of Life Power® cells
Life Power® P1
Life Power® P2
K2 Energy Solution - www.k2es.com

K2 Energy Solutions new 12V 6.4 & 9.6 Ah batteries
•Designed for medical, military, industrial fields
+ consumer applications
K2B12V7
K2B12V10
Backward compatible with lead acid batteries !

Uncompromised quality key to success
Source: SAFT 11th Electrochemical Power Sources R&D Symposium (July 2009)
Minimal impedance growth !

How does LiFe Power® LFP compare to NCA ?
Capacity (Ah)
10
8
6
4
2
0
NCA 100% DOD
NCA 80% DOD
LiFePO 4 100% DOD
"If one want to achieve the same life cycle as
LFP, DOD have to be reduced to 80% for NCA,
which nearly compensates for the energy density
gap between both chemistries on cell level"
0 500 1000 1500 2000
Cycles
Any hesitation for your HEV batteries ?

H2O uptake (ppm)
C-LiFePO4 and its relationship to humidity ...
700
600
500
400
300
200
100
0
0 500 1000 1500 2000
time (second)
But leads to irreversible
chemical degradation
=>
=> C-LiFePO4 likes water !
Capacity (mAh/g)
148
147
146
145
144
143
142
141
Fresh synthesis
1 week aging
at atmosphere
T = 60°C
0 10 20 30
Cycle
40 50
Phostech’s R&D/QC has sensibilized early its customers, allowing them to
introduce suitable technological solution in their battery production line

Capacity (mAh/g)
160
155
150
145
140
135
Activation effect for Life Power® P1
130
60°C
activation
Li/LiPF6 EC-DEC/C-LiFePO4
1 st C/D cycle at 60°C - C/8
2 nd C/D cycle at 60°C - C/8
Cycle
Cycling at 25°C - C/12
0 5 10 15 20 25
Activation suppressed after 60°C cycle !!!

Also positive effect for irreversible capacity ...
Potential (Volt vs. Li + /Li 0 )
4,0
3,5
3,0
2,5
2,0
Li/LiPF6 EC-DEC/C-LiFePO4
1st 1
C/D cycle at 60°C - C/8
st C/D cycle at 25°C - C/12
2 nd C/D cycle at 25°C - C/12
(after 1 st C/D cycle at 60°C - C/8)
0 50 100 150 200
Capacity (mAh/g)
60°C cycle could improve battery performance

Optimization through P1 & P2 mixture
Easier to process than pure P2
Better power than pure P1
Improved packing density/energy density
Excellent cycling stability
Lower resistance
P1/P2 mixture is
a simple solution
Best of both world solution !

Phostech investment in quality
St-Bruno dry room dedicated to QC

Phostech investment in quality
St-Bruno QC cycling facility and laboratory

Automotive QC requirements
Exemple: Life Power® P2 Stoichiometry (at.%) QC
190 consecutive lots including off-spec
Automotive requirements with > 25 parameters to control !!!
Huge QC investments to enter automotive market

Phostech C-LiFePO4 is used and evaluated by
numerous companies (PT, HEV, PHEV, EV, UPS...)
Phostech Lithium
US
Interim Report 2007
Süd-Chemie Group continues successful
performance and exceeds expectations
– Revenue increased 14% compared
with first half of 2006
- – ebit rose 64% compared with first half of 2006
- – Significant upturn in forecast for the full year
Europe
High Energy Large Prismatic Rechargeable Cell
Lithium Nickel Cobalt Manganese (NiCoMax)
China
Others customers disclosed in the coming months ...
World Class. American Made.
Japan
International Battery, Inc.’s Lithium Nickel Cobalt Manganese
rechargeable cells are available in a rugged prismatic format in
capacities ranging from 50 - 200Ah. The thermal stability and safety
Korea
performance of the NiCoMax electrochemical system is superior
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packaging. IB’s cells offer a low self-discharge rate and have excellent
operating temperature characteristics. The excellent thermal stability
and safety performance of the NiCoMax electrochemical system is well
suited for variety of commercial, military and industrial applications.
Features: �����������������������������������������
Applications: �����������������������������������������������������������
applications, communications, backup power, energy
storage (wind, solar, tidal).
NiCoMox Packaged Cells
������������ Condition IB-B-CHE-50 IB-B-CHE-90 IB-B-CHE-200
Nominal Voltage (C/3) 3.7 Volts 3.7 Volts 3.7 Volts
Nominal Capacity (C/3) 50 Ah 90 Ah 200 Ah
�������������� (C/3) 185 Wh 333 Wh 740 Wh
�������������� (C/3) 123 Wh/Kg 135 Wh/Kg 133 Wh/Kg
Peak Power (60% DOD) 30 sec, 2/3 OCV, 60% 675 W (450 W/Kg) 1300 W (517 W/Kg) 3000 W (540 W/Kg)

Multicore "Material" Intellectual Property
1 2 3
Ca
de
Core 1: LiFePO4 (HQ/UT)
US 5,910,382 C1 US 6,514,640 C1
CA 2,251,709 EP 0904607
Core 2: Carbon deposit 1
(ACEP, UdM, CNRS co-ownership)
US 6,962,666 US 7,344,659
EP 1049182 EP 1796189
CA 2,307,119
+ JP examination
Core 3: Carbon deposit 2
(HQ, UdM, CNRS co-ownership)
Necessary "free to operate" LiFePO4 material IP
2 nm
US 7,457,018
KR 100879839
CN 100421289
+ JP, EP and CA examination

Phostech’s improved solid-state C-LiFePO4
Capacity (mAh/g)
180
160
140
120
100
80
60
40
20
0
0
C/10
157 mAh/g
C
136 mAh/g
10C
90 mAh/g
0,1 1 10 100
C-Rate
Performance still improved, sampling in 4Q 2010

Thank you for your attention !
See you next time in Cannes !
For more
information:
info@phostechlithium.com
www.phostechlithium.com