EL-CELL ECD-3 User manual

© 2017 EL-CELL GmbH
© 2022 EL-Cell GmbH
User Manual
Release 1.6
Electrochemical dilatometer
ECD-3

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User Manual ECD-3
Release 1.6
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 product.
EL-Cell GmbH
Tempowerkring 8
21079 Hamburg - Germany
phone: [phone]
fax: [phone]
e-mail: [e-mail]
web: www.el-cell.com

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User Manual ECD-3
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Content
1 Product description ...................................................................................................................................... 4
2 Features............................................................................................................................................................ 7
3 Technical data ................................................................................................................................................ 7
4 Safety Precautions......................................................................................................................................... 8
5 Unpacking........................................................................................................................................................ 8
6 Start-up and disassembly..........................................................................................................................11
7 Assembling the cell inside the glove box .............................................................................................19
8 Further assembly outside the glove box ...............................................................................................27
9 EC-Link Software Installation ...................................................................................................................31
10 Calibration and Settings..........................................................................................................................31
11 Recording the Displacement Signal with an External Potentiostat .............................................31
12 Using the Reference Electrode ........................................................................................................33
13 Using the valve ....................................................................................................................................34
14 Choosing the appropriate spacer disc ..........................................................................................35
15 Dilatometer Disassembly and Cleaning ........................................................................................36
16 Care Instructions .................................................................................................................................37
17 Consumables ........................................................................................................................................37
18 Spare Parts ..................................................................................................................................................38
19 Connector and Cable Pin-out ................................................................................................................44
20 Technical support......................................................................................................................................47
21 Warranty ......................................................................................................................................................47

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User Manual ECD-3
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1 Product description
The ECD-3 electrochemical dilatometer measures charge-induced strain (expansion and
shrinkage) of electrodes down to the nanometer range. The ECD-3 has been mainly developed
to investigate battery and other insertion-type electrodes. It may, however, also be used for
many other electrochemical systems utilizing aprotic organic electrolyte solutions. The
electrode materials can be either bound film or single crystals/grains (e.g., graphite flakes).
The maximum sample size is 10 mm x 1 mm (diameter x thickness).
The heart of the ECD-3 is an electrochemical cell, hermetically sealed against the ambient
atmosphere. The two electrodes inside are separated by a stiff glass frit. The upper working
electrode (WE) is sealed using a thin metal foil, through which any charge-induced thickness
change is transmitted toward the sensor/load unit above. This working principle allows
determining the height change of the working electrode without any interference from that of
the counter electrode (CE).
A high-resolution displacement (LVDT) transducer detects dimensional changes of the WE
ranging from 100 nanometers up to 500 micrometers during the same experiment that may
last a few minutes to many days.
The ECD-3 features an integrated USB data logger for recording the electrode displacement,
temperature, cell potentials, and current. Analog outputs of displacement and temperature are
provided for integration with external instruments.
The dilatometer will be operated inside a temperature-controlled chamber for best accuracy
and drift stability.
Sensor
Membrane
Current collector
T-Frit
WE (working electrode)
CE (counter electrode)
Current collector
REF
Load

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The basic structure of the ECD-3:
Sensor unit
Details shown on the following page
Cell body
Bracket

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Cut drawing of the ECD-3:
LVDT sensor
Flexure
Load
Sensor Tip
Reference electrode
Piston
Micrometer screw
Sensor plunger
Excenter
Locking screw
Spacer disc
Glass-T-Frit
Shut-off valve

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2 Features
The ECD-3 is an electrochemical dilatometer for measuring changes in the thickness of the
working electrode of a battery test cell. The main features of the ECD-3 are briefly described
in the following:
▪LVDT sensor system with <50 nm resolution, drift stability of <100 nm/hour (sample-free
instrument at constant temperature), and 500 µm full range.
▪Conditioning electronics with analog output signals (-10 to 10 V) for displacement and
temperature.
▪Integrated USB data logger for recording displacement, temperature, cell potentials, and
current.
▪3-electrode electrochemical cell
▪Materials in contact with electrolyte: PEEK, borosilicate glass, stainless steel 316L for
aprotic, gold for aqueous electrolytes
3 Technical data
▪Working (upper) electrode: bound electrode film or single crystal/grain; max. sample size
10 mm x 1 mm (diameter x thickness)
▪Counter (lower) electrode: 12 mm diameter
▪Load on a working electrode: 1 N
▪Electrolyte volume: approx. 0.5 ml
▪Operating temperature range: Cell and sensor: -20 to +70 °C;
Conditioning electronics and data logger: 0 to +40 °C
All measurements in mm

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4 Safety Precautions
Use proper safety precautions when using hazardous electrolytes. Wear protective glasses and
gloves to protect you against electrolytes that may accidentally spill out of the instrument
during filling, operation, and disassembly.
5Unpacking
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.
List of Components:
1. ECD-3 dilatometer ECD3-00-0001-A, assembled
2. Box ECD-3 ECE1-00-0006-E, assembled
3. ECD sensor cable ECE1-00-0036-A
4. ECD-3 cell cable ECE1-00-0033-F, assembled
5. Power supply 15W/24V DC ELT9045
6. Power supply adapter ELT9078
7. USB cable type A/B (2.0 m) ELT9167
1
2
3
4
5
6
7

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8. USB stick containing EC-Link data logger software ECE1-00-0052-B
9. Allen wrench 2.5 mm WZG9059
10. Allen wrench 3 mm WZG9058
11. 3 x PE Seal II ECD-3 piston ECC1-01-0044-D
12. 3 x PTFE Seal ECD-3 piston ECC1-00-0044-C
13. 1 x PTFE Seal ECD 33.3 x 1.8 mm (3 pcs.) ECC1-01-0043-D/3
14. 3 x O-Ring 33 mm x 1.78 mm DIC9034
15. 3 x O-Ring 50.5 mm x 1.78 mm DIC9038
16. T-Frit 10/12.5 ECC1-00-0041-B
17. Stiff Plate ECD1-00-0041-A
18. 3 x Ferrule 1.5 mm (short top part) ECC1-00-0029-H
19. Membrane (aprotic) 1.4404 ECC1-00-0019-D
20. Spacer disc Set 2.1 –2.7 mm (3 pcs) ECC1-01-0374-AF
21. Separator (GF/A) 12 mm x 0.26 mm (10 pcs) ECC1-01-0012-Q/X
22. Demonstration kit for ECD ECD1-00-0900-A
11
12
13
8
10
9
14
15
16
18
19
20
21
22
23
24
25
26
27
28
17

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23. Allen wrench set (0.9 / 1.3 / 1.5 / 2) (4 pcs) ECC1-01-0028-A
24. Open end wrench AF7 ECC1-09-2037-A
25. Disassembly device piston ECC1-09-3048-A
26. Allen screwdriver 2.5 mm WZG9003
27. Spherical Allen screwdriver 3 mm WZG9002
28. Tweezer antiacid / stainless WZG9001

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6Start-up and disassembly
Follow the same procedure beginning at step 3 when disassembling the instrument after
completing an experiment.
General advice: Practice the assembly procedure outside the glove box with dummy
components before going for the experiment. Make sure you have understood the how and
why of every single step. Ask us otherwise.
6.1After unpacking the ECD-3, remove the
transport lock from the sensor unit.
6.3Unscrew and detach the sensor unit.
6.2Unscrew the two inner screws first,
only then the two outer screws.

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6.4Screw off the cell body from the
bracket.
6.5Unscrew the spring load from the cell
body.
6.6 Unscrew the reference electrode.
6.7Remove the cover flange.

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6.8When dissassembling the dilatometer for
the first time, remove the stiff plate below the
cover flange. This plate is for transport only.
For the actual experiment, replace the plate by
the provided metal membrane.
6.10 Now the frit flange with the PTFE-
Seal and the piston in the middle are
visible.
6.9 Remove the stiff plate or membrane
from the cell body
6.11 Pull the frit flange out of the cell body.

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6.12 Loosen the socket screw at the end of
the piston a little with the Allen wrench
(half turn). This releases the disk springs
inside piston and allows it to be pulled
out.
6.13 Pull the piston out of the frit flange
by using the dedicated removal tool.
To do this, first, screw the two halves of
the tool together.
6.14 Insert the frit flange with inserted
piston from below.

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6.15 Slide the locking disc completely over
the tool as shown in the picture.
6.16 Unscrew the tool to remove the
piston from the frit flange.

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6.17 Remove the socket screw at the end
of the piston and disassemble it. Both
seals need to be renewed before each test.

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The following steps 6.18 to 6.20 describe the disassembly of the base body, dead volume
cover, and dead volume valve. The dead volume option is no longer used with the updated
version of the dilatometer. Therefore, leave those parts in the assembled state. The valve does
not need to be installed.
6.18 Remove the dead volume cover and
both O-rings.
6.19 Unscrew the valve stem and the valve
body.
6.20 Remove the three screws that fix the
dead volume cover.

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With the updated version (2022) of the dilatometer, the dead volume and valve (comprised of
items 5, 6, 11, 12, 15, and 16) can always be left in the assembled state. There is no need for
cleaning and drying these parts before use. The valve does not need to be installed.
All other parts must be dried before moving into the glove box for assembly. Recommended
drying conditions: 80°C, <0.01 mbar, 12 hours.
NOTE: For highly moisture-sensitive systems, we recommend drying the glass frit separately at
a higher temperature: 180°C, <0.01 mbar, 12 hours.
1.Membrane (aprotic) 1.4404
2.Spacer disc (proper thickness depends
on working electrode thickness)
3.T-frit
4.Cover the flange with three screws
5.Dead volume cover with three screws
6.ECD-3 base body
7.Frit flange
8.Spring load
9.Reference electrode
10.Piston PTFE-sealing, internal thread
(ECD-3)
11.O-Ring 50.5 x 1.78 mm, EPDM
12.O-Ring 33.05 x 1.78 mm, EPDM
13.Socket screw
14.PE-Seal for ECD-3 (33 mm x 1.6 mm)
15.Ferrule 1.5 mm, PTFE
16.Shut-off valve (Note: Not used with
the updated version of the
dilatometer)
17.PTFE Seal ECD-3 piston
18.PE Seal II ECD-3 piston
19.Thrust screw VII (ECD-3)
20.)
1
15
6
8
10
4
5
14
7
2
16
3
9
1
12
13
11
19
20
18
17

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7Assembling the cell inside the glove box
After moving the different parts of the disassembled cell body into the glove box, follow the
steps below. Protect yourself and handle the chemicals with care.
7.1 Inside the glove box: Insert the T-frit
with the smaller side pointing downwards
into the frit flange.
Note: Make sure that the inside of the frit
flange does not get damaged/ scratched
when inserting the T-frit. Replace the frit
flange as necessary.
7.2 Inside the glove box: Put a glass fiber
separator (12 mm diameter) on top of the
frit
7.3 Inside the glove box: Insert the
lithium metal counter electrode.

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7.4 Inside the glove box: First place the
PE sealing (PE Seal II ECD-3 piston)
followed by the PTFE sealing (17.PTFE Seal
ECD-3 piston) on the piston. The outward
curved side of the sealing rings must face
away from the piston (see sketch below)
7.5 Inside the glove box: Add the thrust
screw.
Align it so that the mark on the thrust
screw is centered on the recess in the
piston.
7.6 Inside the glove box: Tighten the
socket screw gently with the provided
allen wrench.