EL-CELL ECC-Press-Air, ECC-Press-Air-DL User Manual

© 2012 - 2017

EL-CELL GmbH

Electrochemical Test Cell

ECC-Press-Air (-DL)

User Manual

Release: 1.5

2017-06-12

Page 2 of 23 Manual_ECC_PRESS_AIR_Release 1.5.docx / 13.06.2017

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.

Content

1 Product Description .......................................................................................... 3

2 Features and Specification .............................................................................. 3

3 Safety Precautions ........................................................................................... 7

4 Unpacking ........................................................................................................ 7

5 Cell Assembly .................................................................................................. 8

6 Operation Modes / Gas Supply ...................................................................... 11

7 Electrical Connection ..................................................................................... 11

8 Sample Valve with Septum Port .................................................................... 13

9 Software Installation (DL option) .................................................................... 14

10 Recording the Pressure Signal with an External Potentiostat ........................ 15

11 Disassembly and Cleaning ............................................................................ 16

12 Accessories and Spare Parts ......................................................................... 17

13 Cables and Connectors ................................................................................. 21

14 Technical Support ......................................................................................... 22

15 Warranty ....................................................................................................... 23

EL-CELL GmbH

Tempowerkring 8
D-21079 Hamburg - Germany
phone:[phone]
fax: [phone]

[e-mail]
www.el-cell.com

Page 3 of 23 Manual_ECC_PRESS_AIR_Release 1.5.docx / 13.06.2017

1 Product Description

The ECC-Press-Air test cell is dedicated to the characterization of gas diffusion
electrodes in aprotic electrolytes, in particular for lithium-air batteries. The attached
pressure sensor serves to monitor the inside pressure in either a flow-through or in a
dead-end pressurized set-up. The ECC-Press-Air combines all the features of the
ECC-Press and the ECC-Air test cells.

The provided low-dead-volume sampling port/valve serves to draw gas samples from
the cell’s headspace. The cell hardware is based on the ECC-Std and ECC-Ref test
cells and can be used with or without a reference electrode.

The ECC-Press-Air comes with a controller box for easy interfacing with an external
potentiostat. The box provides analog outputs for both pressure and temperature. As
an option, all relevant signals of the experiment – cell pressure, temperature, cell
potentials and current – may be recorded with an integrated USB data logger (DL
option).

Pressure sensor 0 to 2.5 bar abs.

Variable dead volume by means of
two sensor spacers

Stand (wall mountable)

Port (plugged or for
gas outlet)

Sampling valve with
syringe port or port
for gas inlet

Reference pin

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2 Features and Specification

 ECC-Press-Air test cell dedicated to the characterization of gas-diffusion

electrodes in aprotic media

 Upper electrode is contacted by, and breathes through a perforated current

collector

 Gas inlet and outlet for supply of pressurized gases to the gas diffusion

electrode

 A siphon directs the incoming gas to the backside of the gas diffusion

electrode

 Sampling valve with septum port for drawing gas samples by means of a

syringe

 Attached pressure sensor for monitoring of inside gas pressure. Default

pressure range of 0 to 2.5 bar (absolute).

 Conditioning electronics with analog outputs for pressure and temperature for

seamless integration with external instrumentation

 Total dead volume variable between 4.45 cm3 (both sensor spacers in place)

and 16.92 cm3 (without spacer)



Dead volume in cm3

1. Both spacers installed*

4.45

2. Only ECC1-00-0136-A (sensor spacer B) installed**

10.58

3. Only ECC1-00-0135-A (sensor spacer A) installed**

10.78

4. No spacer installed**

16.92

* delivery condition

**Requires de-mounting of the sensor and must be done at factory.

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 Optional integrated USB data logger for recording of cell pressure,

temperature, cell potentials and current (DL option)

 Operation in either flow-through or dead-end pressurized set-up
 Fully equipped for operation with and without reference electrode
 Reliable ultra-low leakage sealing with PE seal
 High precision 18 mm diameter sandwich geometry with <0.1 mm electrode

concentricity

 Operating temperature range -20 to +70°C (cell)
 Easy and reliable electrolyte filling upon assembly
 Fast assembly and dismantling, and easy cleaning of cell components
 Electrodes are easily accessible for post-mortem analysis
 Reusable cell components except for PE seals
 Small and defined electrolyte volume down to 0.05 cm3
 Adjustable, reproducible and homogeneous mechanical pressure on

electrodes

 Materials in media contact are stainless steel 1.4404 and PEEK (other

materials on request)

 Modular cell construction with many interchangeable components
 Size (including stand): 90 mm x 80 mm x 240 mm (height x width x depth)
 Weight: 900 g
 Dedicated tools available to ease cell assembly and operation

http://el-cell.com/products/accessories-tools

Dimensions (Cell)

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Electrical Specifications (Controller)

- Input: 24 V (0.6 A) supplied by PSA15R-240P mains adapter

- Analog output voltages: 0 to 10 V (1 kOhm / 100 nF) for pressure and
temperature

- Resolution of pressure analog output: <0.05% of measurement range

- Error of pressure analog output: <0.5% of measurement range (comprising
non-linearity including hysteresis and non-reproducibility)

- Resolution of temperature analog output: <0.01°C

- Error of temperature output: < 1°C

- Optional USB data logger powered by host PC with galvanic isolation

- Operating temperature range (controller): 0 to 40°C

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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 filling and disassembly. Upon cell disassembly,
dispose all materials properly. Metallic lithium and some insertion compounds may
decompose heavily 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 components. Contact the factory if anything is missing or
damaged. NOTE: Damaged shipments must remain with the original packaging for
freight company inspection.

List of Components

1. ECC-Press-Air test cell with pressure sensor, assembled for use in a

2-electrode dead-end pressurized set-up

2. Gas sample port with septum and valve

3. Reference electrode pin, REF sleeve and locking pin for 3-electrode

operation

4. PE seals (10 pieces)

5. Septum (10 pieces)

6. One-way syringe and needle

7. Glass fiber separators 18 mm x 1.55 mm (10 pieces)

8. Sleeve removal tool

9. 24 V power supply with country specific adapters

10. Controller box with analog outputs for pressure and temperature, 4 mm

banana sockets for connection to an external potentiostat, and integrated
USB data logger (DL option)

11. CD with manual and data logger software (DL option)

12. USB cable (DL option)

13. Cell cable for connection between test cell and controller box

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5 Cell Assembly

The test cell can either be operated in 2-electrode or 3-electrode (reference)
configuration. In the following, the cell assembly is described for operation with a
lithium metal reference electrode.

Generally, all assembly steps are to be carried out in inert glove box atmosphere,
and all components used are to be dried upfront in a vacuum oven at 80°C for at
least 12 hours. The pressure sensor together with the transfer line may remain
permanently attached to the stand.

In order to operate the test cell with a reference, the small feed-through hole of the
REF sleeve is to be loaded with the reference material, usually metallic lithium. The
vertical position of the reference is determined by the thickness of the components.
Make sure that the electrodes
and separator used have the
appropriate thickness to avoid
a short circuit between the
reference and anyone of the
two other electrodes. The
smaller (inside) diameter of
the reference bore is 0.3 mm.

Assembly Steps:

i) Make sure that the siphon is properly attached to the cell lid. For this purpose,

plug the siphon into the cell lid with the siphon side bore pointing to the gas
outlet port in the lid. Then attach the tube (transfer line) to the gas outlet port
so that the tube end fits into the side bore and thus holds the siphon in place.

ii) Pick up a small piece of lithium by a metal wire, and press the lithium into the

feed-through hole of the REF sleeve until the lithium just arrives at the inner
face of the sleeve. Note that significant force has to be applied to achieve that.
A special REF loading tool is available for this purpose (not included).

iii) Close the side opening of the cell base with the provided plug. This plug is

later on replaced by the reference pin.

iv) Assemble the two-part WE piston with the perforated current collector pointing

upwards

v) Insert the WE piston into the sleeve with the perforated current collector

pointing upwards.

vi) Put the 18 mm diameter gas diffusion electrode onto the piston inside the

sleeve.

Separator

Lower Electrode

Upper Electrode

Separator

Lower Electrode

Upper Electrode

Separator

Lower Electrode

Upper Electrode

0.9 mm

Separator

Lower Electrode

Upper Electrode

Separator

Lower Electrode

Upper Electrode

Separator

Lower Electrode

Upper Electrode

Separator

Lower Electrode

Upper Electrode

0.9 mm

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vii) Put the glass fibre separator into the sleeve and dispense a defined amount of

electrolyte onto it. The optimum amount of electrolyte depends on the
electrodes and separator used, and has to be carefully determined in pre­tests. 0.5 cm3 are a reasonable amount for 1.5 mm thick glass fiber separator.

viii) Put the lithium CE disc (18 mm diameter, approx. 0.2 mm thick) on top of the

cell stack.

ix) Push the cell base over the assembly, hold the components tightly together,

and turn the assembly back into the upright position.

x) Release the pressure applied on the cell stack, mount the locking ring to align

the side opening of the cell base with the feed-through hole of the REF sleeve,
and replace the plug in the cell base by the spring-loaded REF pin.

xi) Insert the PE seal and the spring.
xii) Attach the cell lid with the siphon and tube already attached
xiii) Push the cell into the bracket, and tighten the wing nut.

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Lid with 2mm
banana jacks

Wing Nut

Siphon

Connection line to
pressure sensor

Gas inlet or gas
sample port / valve

Locking ring

Piston

PE seal

REF sleeve

Cell base with 2mm
banana jacks

Spring

Cell stack

Perforated current

collector

Reference assembly

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6 Operation Modes / Gas Supply

Thanks to its modular design, the ECC-Press-Air may be operated in different
modes. Two basic set-ups are described below.

A. Flow-through set-up
This is the most typical configuration for the characterization of Li-air batteries. In the

simplest set-up of this kind, the cell inlet is connected to the gas (oxygen) supply via
a mass flow controller, and the pressure build-up inside the cell is controlled by
means of a metering valve (or narrow capillary) at the gas outlet located at the sensor
adapter. For gas analysis, the gas outlet may be connected to the "continuous" gas
flow inlet of a mass spectrometer. A small dead volume and plug flow conditions are
mandatory for a good time-resolution of the gas analysis. This is achieved by having
all spacers installed inside the test cell and in the sensor adapter. Even better time
resolution is possible with the ECC-DEMS test cell.

B. Dead-end pressurized set-up
In this configuration, the gas outlet at the sensor adapter is plugged, and the test cell

is pressurized at the beginning of the experiment through the attached sample valve/
port. After equilibration of the closed cell at constant temperature (the time constant
mainly determined by the slow dissolution of gases in the electrolyte), the cell is
charged/ discharged and the resulting pressure change is recorded. For a given
amount of gas, the magnitude of pressure change is the larger, the smaller the dead
volume. The gas composition may be analysed by drawing gas samples via the
attached sample valve/ port. However, for gas analysis, the dead volume spacer in
the sensor adapter must be in place in order to avoid concentration gradients.

7 Electrical Connection

For best results, place the ECC-Press-Air inside a temperature controlled chamber,
at a constant temperature between -20 to +70°C. The chamber needs to have a feed­through for cable connection to the controller box outside the chamber.

Inside the chamber, attach the square sensor plug to the pressure sensor, and
connect the 2 mm banana plugs of the cell cable to the cell (red and green to the lid,
blue and yellow to the base, black to the reference).

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Outside the chamber, connect your potentiostat to the 4 mm banana sockets on the
front panel of the controller box. The rightmost column in the table below refers to the
terminology used for the lead connections of Biologic potentiostats (MPG-2, SP, VSP
and VMP series).

Both the pressure and the temperature signals are available at the Analog Out
connector of the controller box. These signals can either be routed to the analog
inputs of the controlling potentiostat (if available), or to some other recording device.

The pressure is linearly related to the pressure sensor voltage according to
P(abs) = 0.25 bar/V * Voltage

Likewise, the temperature is related to the temperature sensor voltage according to
T = 8°C/V * Voltage

Controller

Box

Potentiostat

Biologic Potentiostat

VSP, VMP3 etc.

I1

WE Current

WE

V1

WE Sense

Ref1

REF

Reference

Ref2

V2

CE Sense

Ref3

I2

CE

CE

GND

GND

GND

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8 Sample Valve with Septum Port

The gas sample valve serves to draw gas samples from the head space of the ECC­Press-Air test cell. In the closed state, the valve spindle is seated on the PTFE ferrule
and is thus preventing any bleeding from inside the cell through the septum. In order
to draw a gas sample, i) pierce the septum with the sample syringe, ii) open the valve
by turning the valve handle counter-clockwise by 90 degrees, iii) charge the syringe,
iv) close the valve by turning the valve handle clockwise till finger tight, and remove
the syringe.

Valve Seating

PTFE Ferrule

Valve Handle

Septum Port

Septum

Valve Stem

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9 Software Installation (DL option)

The ECC-Press-Air-DL features an integrated USB data logger for recording cell
pressure, temperature, cell potentials and current. The software installation on a

Windows® PC is described below.

a. You must be logged into an account with Administrator privileges.
b. Save your work and close down all active programs.
c. On the installation CD, run X:\setup. This will install the EC-Link data

logger software. Follow any instructions that may appear on your screen.

d. Once installation is finished plug in the provided USB cable into both the

host PC and the ECC-Press-DL controller box.
e. Launch the data logger software if not already done.
f. After a few seconds, the data logger software should report a valid

connection and you are ready to start the measurement.

Additional information on the EC-LINK software can be found in the EC-LINK Quick
Start Guide.

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10 Recording the Pressure Signal
with an External Potentiostat

Many of today’s battery testers and potentiostats provide additional analog inputs
that may be used to record sensor signal along with cell current and potential.

In the following, the combination of the ECC-Press-Air-DL with a Biologic potentiostat
(MPG-2, SP, VSP and VMP series) is described as an example. The Biologic
potentiostats feature two analog inputs that are used here to record both pressure
and temperature.

1. Connect the 9-pin Sub-D connector of the optional analog output cable to the
analog input of the respective Biologic VMP3 channel.

2. Launch the EC-Lab software.

3. From the ECC-Press-Air documentation CD, load the EC-Lab setting file ECC­Press.mps.

4. In the External Devices dialog, click on Record external devices to see the
settings applied to the analog inputs.

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11 Disassembly and Cleaning

Right after use, disassemble the cell in the reverse order of assembly. Note that the
reference pin MUST be detached before the REF sleeve can be removed.
All chemicals used have to be disposed properly. All wetted parts are to be
cleaned with water and/or other appropriate solvents. Ultrasonic cleaning is
recommended. Persistent dirt on the cell base and plunger may be removed by
treatment with aqueous nitric acid (20%, 2 hours at room temperature). All parts are
to be dried immediately after cleaning at 80°C.
It is recommended to leave the pressure sensor together with the transfer line
attached to the stand. Typically, these parts need not be disassembled or cleaned.

NOTE: Leaving cell parts in contact with ambient atmosphere while still being wetted
with electrolyte may result in severe corrosion.

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12 Accessories and Spare Parts

ECC-Press-Air (-DL)
complete

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Test Cell

(assembled as 3-electrode cell)

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Gas sample port, assy
ECC1-00-0155-A

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Reference pin, assy
ECC1-00-0010-D

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13 Cables and Connectors

Cell Cable

6x2 twisted pairs; Sub-D M15 HD connector to box; 2 mm banana plugs and square
sensor plug M16 to ECC-PRESS test cell; shield connected to Sub-D connector
housing and to sensor housing; Pt100 sensor located inside sensor plug housing

Part No. ECE1-00-0032-B

Biologic VMP3 Auxiliary Cable (2 x 2 x 0.14 mm

2

, TP, shielded)

Sub-D F9 connector to box; Sub-D M9 connector to auxiliary input connector of the

Biologic potentiostat. The cable shield is tied to both connector housings.

Part No. ECE1-00-0040-B

Pin #

Signal

Cable Color

Comments

1

V1

Red

Red plug

2

V2

Blue

Blue plug

3

4 REF

Grey

Grey plug

5

I2

Yellow

Yellow plug

6

7 8 9

10

I1

Green

Green plug

11

Pt100 (1)

Violet

Pt100 sensor inside

sensor plug housing

12

Pt100 (2)

Black

13

+24V

White (1)

Square sensor plug

14

Sensor-I

Brown (2)

15

Sub-D HD F15 to box

Sub-D M9 to Biologic AUX Input

Pin #

Signal

Cable Color

Pin #

Signal

Comments

1 2

T (VTEMP2)

Green

6

Analog In 2

0..10V; 8°C/V

3 4 5

P (VP2)

White

1

Analog In 1

0..10V; 0.25 bar/V

6

7

8

9 GND

Brown

7

GND

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14 Technical Support

Technical support for this product is exclusively handled by EL-CELL GmbH.
The following procedure must be followed when the ECC test cell or any part of it is
returned to EL-CELL GmbH for repair:

1. Send an e-mail to [e-mail] to obtain a return authorization number

and a decontamination report form.

2. Sign the decontamination report asserting that the instrument has been

decontaminated and is safe for technicians to work on it.

3. Describe in detail what is wrong.

4. Include a contact name, address, telephone number, and email address.

5. Return the equipment to

EL-CELL GmbH
Tempowerkring 8
D-21079 Hamburg
Germany
Email [e-mail]

Page 23 of 23 Manual_ECC_PRESS_AIR_Release 1.5.docx / 13.06.2017

15 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 labour,

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 centre. 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 shall
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 signed by the parties hereto.