EL-CELL ECC-PAT-Core, ECC Series User Manual

© 2016 EL-CELL GmbH
User Manual
Rel ease 2.02
Electrochemical Test Cell ECC-PAT-Core
November 2016
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User Manual ECC-PAT-Core – Release 2. 02
The information in this manual has been carefully checked and believed to be accurate; however, no responsibility is assumed for inaccuracies.
EL-CELL GmbH maintains the right to make changes without further notice to products described in this manual to improve reliability, function, or design. EL -CELL GmbH does not assume any liability arising from the use or application of this p roduct.
EL-CELL GmbH
Tempowerkring 8
21079 Hamburg - Germany
phone: +49 40 79012-737
fax: +49 40 79012-736
e-mail: in fo @e l- ce ll.com
web: www.el-cell.com
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User Manual ECC-PAT-Core – Release 2. 02
Content
1 Product Description ............................................................................................ 4
2 Features ........................................................................................................... 6
3 Safety Precautions ............................................................................................. 6
4 Unpacking ......................................................................................................... 6
5 Cell Assembly .................................................................................................... 8
6 Different Test Cases .......................................................................................... 10
7 PAT-Core Components ....................................................................................... 11
9 Disassembly and Cleaning .................................................................................. 14
10 Consumables ................................................................................................... 14
11 Spare Parts ..................................................................................................... 15
12 Technical Support ............................................................................................ 16
13 Warranty ........................................................................................................ 17
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12
12,2
12,4
12,6
12,8
13
13,2
13,4
13,6
13,8
14
0 200 400 600 800 1000
SPRING FORCE APPLIED ON CELL STACK / N
THICKNESS OF UPPER ELECTRODE / MICRONS
1 Product Description
The ECC-PAT-Core is the latest test cell of the ECC series, which allows the application of the novel PAT-Core. The PAT-Core is comprised of three components:
1. Insulation sleeve: The polypropylene insulation sleeve with a ring -shaped
reference electrode and a separator, both pre-installed at the factory, sealed and ready for use in the glovebox. Several other versions are available for special purposes. The insulation sleeve is also available in the disassembled state, so that the customer can use his own separator or reference .
2. Lower plunger: The lower plunger serves as the positive current collector.
Different gap sizes are available to match electrodes and separators with different thicknesses. When using the proper gap size, the lower electrode ca n have a maximum thickness of 800 µm.
3. Upper plunger: The upper plunger serves as the negative current collector. The
maximum thickness of the upper electrode is 800 µm. Note that the spring force applied on the cell stack will depend slightly on the thickness of the upper electrode.
4.
Spring force in relation to the thickness of the upper electrode:
Compression sp ring FED9015
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The insulation sleeve is a single -use component, which has to be disposed after use. In contrast, the plungers are available as both single -use components (made of battery grade copper and aluminium) and as reusable components (made of stainless steel 316 L/ 1.4404).
Ins ulation sle eve
Upp er plunger
Low er plunger
PAT -Core
ECC-PAT-Core
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2 Features
The ECC-PAT-Core is a test cell to accurately characterize aprotic lithium-ion battery materials over long periods of times. The standard PAT-Core is composed if a lithium metal ring and a a separator (either glass fiber or a nonwoven polyester pasted with Al2O3). Both the reference and the separator are pre-installed in a single-use insulation sleeve. This concept has got several advantages:
Ability for conducting long-term mea surements with a reliable reference electrode
over more than one thousand hours of battery operation .
Ability for measuring half cell impedance spectra throughout the battery’s life
time.
Less mistakes that may result from corrosion or cross-contamination. Increase of testing productivity by single -use concept. No need for cleaning or drying cell components. Fast assembly and dismantling lowers lead times of experiments. Easy and reliable electrolyte filling upon assembly (defined electrolyte volume
dow n to 0.05 cm³).
Reliable leakage-proof sealing with PE-Seal and double cutting ring. Reproducible a nd homogeneous mechanical pressure on electrodes . High precision 18 mm diameter sa ndwich geometry with a concentricity better
than 0.1 mm (electrode and separator dimensions are compatible with other test cells of the ECC series).
The ECC-PAT-Core is designed for use in the temperature range from -20 to +70°C.
3 Safety Precautions
Use proper safety precautions when using hazardous electrode materials and electrolytes. Wear protective glasses and gloves to protect you against electrolyte that may accidentally spill out during disassembly. Upon cell disassembly, dispose all materials properly. Metallic lithium and some insertion compounds may decompose hea vily in contact with water and other solvents, and can cause fire.
4 Unpacking
Check the contents of the packages against the list given below to verify that you have received all of the required components. Contact EL-CELL, if anything is missing or damaged. NOTE: Damaged shipments must remain within the original packaging for freight company inspection .
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List of Components:
ECC-PAT-Core test cell without PAT-Core
Note: The components of the PAT-Core (insulation sleeves and plungers) must be purchased separately.
Lid
PE-Se al
Cell Base
Feed wire assy
Bra cket
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5 Cell Assembly
This section describes, how the ECC-PAT-Core has to be assembled in order to conduct proper battery tests. Please note that the assembly has to take place under the protective atmosphere in a glove box.
1. Put the insulation sleeve (5) onto the worktop with the smaller side pointing
upwards. Different insulation sleeves are available for different test purposes, see chapters 6 and 7.
2. Insert the lower electrode ( 6) into the sleeve with the active layer facing
dow nwards.
3. Attach the lower plunger (7). The lower plunger is available in different gap
sizes in order t o account for the thickness of the electrodes and separator used, see chapters 6 and 7.
4. Turn the assembly upside down.
5. Align the contact spring of the sleeve with the horizontal contact pin inside the
cell base (9). Then insert the assembly into the cell base .
6. Eve nly dispense 100 µL of electrolyte (4) on top of the separator with a pipette.
Note: The optimum amount of electrolyte will depend on the thickness and porosity of the separator and the electrodes used.
7. Insert the upper electrode ( 3) into the insulation sleeve with the active layer
facing downwards.
8. Attach the upper plunger (2).
9. Mount the PE-Seal (8) on the cell.
10. Put the lid (1) (with integrated spring) on top .
11. Hold the lid down and push the cell into the bracket (11).
12. Turn the wing nut (10) to close the cell.
A video showing the assembly of the ECC-PAT-Core in detail, can be found here.
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Lid
Upper plunger
Upper electrode
Ele ctr olyte
Insulation sle eve
Low er electrode
Low er plunger
PE-Se al
Cell base
Bra cket
Win g nut
Further recommended tools for working with the ECC-PAT-Core:
ECC1-02-0005-A ECC-LiPunch 18 mm
ECS1-00-0100-A EL-Cut Cutting Pliers 18 mm
1
3 4 5 6 7 8 9
10
11 2
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6 Different Test Cases
The PAT-Core may be used for many different battery and capacitor types . The table below summarizes some of the most common test cases. In general, we recommend sleeves with built-in glass fiber separator rather the n thin technical separators (such as Viledon or Celgard) when lithium metal is used as the negative electrode, and when measuring half cell impedances.
Battery
Type
Lower electrode
(+)
Upper electrode
(-)
Lower plunger
single-use/re-use
Upper plunger
single-use/re-use
Separator
Li-metal
LCO, NCA, NCM or LFP
Li
Al/SS
Cu/SS
GF
Li-metal
Graphite or silicon
Li
Cu/SS
Cu/SS
GF
Li-metal
LTO
Li
Al or Cu/SS
Cu/SS
GF
Li-ion
LCO, NCA, NCM, or LFP
Graphite
Al/SS
Cu/SS
GF or thin
Li-ion
LFP
LTO
Al/SS
Al or Cu/SS
GF or thin
EDLC
AC
AC
Al/SS
Al/SS
GF or thin
Li-ion cap
AC
Lithiated graphite
Al/SS
Cu/SS
GF or thin
The lower electrode can have a thickness of up to 800 µm provided that the proper gap size of the lower plunger is chosen. The maximum thickness of the upper electrode is
800 µm.
Upp er plunger
Ring-shaped re ference electrode
Ins ulation sle eve
Low er plunger
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7 PAT-Core Components
Lower Plunger:
The lower plunger is available in different materials (SS 1.4404, Al 99.5%, Cu 99.9%) and with different gap sizes. The different gaps are necessary in orde r to account for
the different thicknesses of the lower electrode and the separator used. The term ‘ gap
refers to the distance between the lower face of the built -in separator (thought of as having zero thickness) and the upper face of the lower plunger when attached to the insulation sleeve, see sketch below.
If you use a wrong plunger gap, you may get trouble with your battery test. The below figures illustrate this point.
Good case: No bending of built-in separator; reference ring is in plane with separator.
Gap
Gap too large: Excessive
dow nward bending of built-in separator; reference ring is out of plane with separator.
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Available lower plungers:
The lower plunger is available with gap sizes between 50 and 800 in steps of 50 µm. For ordering, just append the step size to the article code, see table below.
For lower electrodes having a thickness of around 100 µm, we recommend a gap size of 100 when using thin separators such as Viledon or Celgard, and a gap size of 200 when using our standard glass fiber separator. In general, for glass fiber, the gap size must be approx. 100 µm larger than the electrode thickness because of the compression of the built-in separator.
Gap of lower plunger
(in µm)
50
100
150
200
..
800
Article code lower plunger
(SS)
ECC1-01­0027-C_50
ECC1-01­0027-C_100
ECC1-01­0027-C_150
ECC1-01­0027-C_200
ECC1-01­0027-C_800
Article code lower plunger
(Al)
ECC1-01­0027-A_50
ECC1-01­0027-A_100
ECC1-01­0027-A_150
ECC1-01­0027-A_200
ECC1-01­0027-A_800
Article code lower plunger
(Cu)
ECC1-01­0027-B_50
ECC1-01­0027-B_100
ECC1-01­0027-B_150
ECC1-01­0027-B_500
ECC1-01­0027-B_800
Gap too small: Excessive upward bending of built-in separator; reference ring is out of plane with separator.
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Upper Plunger:
The upper plunger is available in different materials: Stainless steel 1.4404, Al 99.5% and Cu
99.9%. Other materials on request.
type of utilization
(single-use vs. reusable)
Art-No. upper plunger copper
Cu 99.9
(E-CU 58)
single-use
ECC1-01-0026-A
aluminium
Al 99.5
(EN-AW- 1050)
single-use
ECC1-01-0026-B
stainless steel
316L
(1.4404)
reusable
ECC1-01-0026-C
Insulation sleeve:
The insulation sleeve is available with and without a ring-shaped lithium metal reference ring, and with two different types of separator: borosilicate glass fiber separator (Whatman GF/A) having a thickness of 260 µm, and nonwoven polyester pasted with Al2O3 (Freudenberg Viledon FS 3005-25) having a thickness of 25 µm. Other separators and customized solutions are available on request. Furthermore, the sleeve is available in the disassembled state, either with or without the lithium reference ring. The table below comprises the four standard versions only.
Art-No.
type of testing
(2 or 3 electrodes)
Insulation sleeve
with lithium metal ring reference,
with glass fiber separator (260 µm)
ECC1-00-0210-O/x
3 electrodes
Insulation sleeve
with lithium metal ring reference,
with Viledon separator (25 µm)
ECC1-00-0210-A/x
Insulation sleeve
with glass fiber separator (260 µm)
ECC1-00-0210-P/x
2 electrodes
Insulation sleeve
with Viledon separator (25 µm)
ECC1-00-0210-B/x
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9 Disassembly and Cleaning
After disassembly, dispose all single-use components and electrodes properly. If the cell base has got contaminated with electrolyte, clean it with plenty of water and dry with compressed air. Use less electrolyte for subsequent tests. Plungers made of stainless steel have to be cleaned with plenty of water. If necessary, remove persistent dirt with aqueous nitric acid (20%, 2 hours at room temperatu re). All other cell components are for immediate re-use without cleaning.
10 Consumables
Plunger (single-use):
Upper plunger (Al) ECC1-01-0026-B Upper plunger (Cu) ECC1-01-0026-A Lower plunger (Al), gap x = 50 to 800 ECC1-01-0027-A_x Lower plunger (Cu), gap x = 50 to 800 ECC1-01-0027-B_x
Insulation sleeves (single-use):
Insulation sleeve with Li-reference ring and Viledon separator
ECC1-00-0210-A/x
Insulation sleeve with Viledon separator only
ECC1-00-0210-B/x
Insulation sleeve with Li-reference ring and glass fiber separator
ECC1-00-0210-O/x
Insulation sleeve with glass fiber separator only
ECC1-00-0210-P/x
Seals (single-use):
Ferrule 1.0 ECC1-00-0029-B PE-Seal (lid)* ECC1-00-0053-A
* W e recomm end r eplacement of the PE-Seal after every u se.
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11 Spare Parts
Components:
PE-Se al
ECC1-00-0053-A
Lid (ECC-PA T-Core)
ECC1-00-0057-M
Sha ft ring
FED9029
Dead volume adapter (ECC- PAT-Core)
ECC1-00-0224-A
Com pre ssion sp rin g (Au)
FED9015
Low er plunger (SS)
ECC1-01-0027-C_x
or Lower plunger (Al)
ECC1-01-0027-A_x
mor e versions see chapter 7
PE-Se al
ECC1-00-0053-A
Cell base
ECC1-00-0056-M
Upper plunger (SS)*
ECC1-01-0026-C
or Upper plunger (Cu)*
ECC1-01-0026-A
Insulation sleeve with bu ilt-in G F
sep arator and wit h Li-ref erence ring
ECC1-00-0210-O/ x
or Insulation sle eve with built-in G F
sep arator (no ref erence)
ECC1-00-0210-P/x
mor e versions see chapter 7
Feed wire assy ( ECC -PAT- Core)
ECC1-00-0010-M
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Plunger (reusable):
Upper plunger (SS)
ECC1-01-0026-C
Lower plunger (SS), ), gap x = 50 to 800 (steps of 50)
ECC1-01-0027-C_x
12 Technical Support
Technical support for this product is exclusively provided by EL-CELL GmbH.
EL-CELL GmbH
Tempowerkring 8
21079 Hamburg - Germany
phone: +49 40 79012-737
fax: +49 40 79012 -736
e-mail: in fo @e l- ce ll.com
web: www.el-cell.com
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13 Warranty
For a period of one year from the date of shipment, EL-CELL GmbH (hereinafter Seller) warrants the goods to be free from defect in material and workmanship to the original purchaser. During the warranty period, Seller agrees to repair or replace defective and/or nonconforming goods or parts without charge for material or labor, or, at the
Seller’s option, demand return of the goods and tender repayment of the price. Buyer’s
exclusive remedy is repair or replacement of defective and nonconforming goods, or, at Seller’s option, the repayment of the price.
Seller excludes and disclaims any liability for lost profits, personal injury, interruption of service, or for consequential incidental or special damages arising out of, resulting from, or relating in any manner to these goods.
This Limited Warranty does not cover defects, damage, or nonconformity resulting from abuse, misuse, neglect, lack of reasonable care, modification, or the attachment of improper devices to the goods. This Limited Warranty does not cover expendable items. This warranty is void when repairs are performed by a non-authorized person or service
center. At Seller’s option, repairs or replacements will be made on site or at the factory.
If repairs or replacements are to be made at the factory, Buyer sha ll return the goods prepaid and bear all the risks of loss until delivered to the factory. If Seller returns the goods, they will be delivered prepaid and Seller will bear all risks of loss until delivery to Buyer. Buyer and Seller agree that this Limited Warranty shall be governed by and construed in accordance with the laws of Germany.
The warranties contained in this agreement are in lieu of all other warranties expressed or implied, including the warranties of merchantability and fitness for a particular purpose.
This Limited Warranty supersedes all prior proposals or representations oral or written and constitutes the entire understanding regarding the warranties made by Seller to Buyer. This Limited Warranty may not be expanded or modified except in writing sig ned by the parties hereto.
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