ECD-3-nano

Electrochemical dilatometer ECD-3-nano

Test cell for the measurement of height changes in aprotic as well as aqueous electrolytes with nanometer resolution


Product news March 2022:

Discover the new ECD-4-nano, the highly improved successor of the ECD-3-nano!

  • Highly improved cycling stability due to redesigned sealing concept
  • Capacitive displacement sensor (range 250 μm, resolution ≤ 5 nm)
  • Additional gas pressure (0 to 3 bar) and temperature sensor (-20 to 80° C)
  • Cableless connection via PAT socket, with electronic cell tag (PAT-Button)
Read more

Watch your electrodes breathing

The ECD-3-nano is the dilatometer with a displacement resolution in the nanometer range. The capacitive parallel-plate sensor systen of the ECD-3-nano can obtain displacement signals of below 5 nanometers. This high resolution makes it possible to explore new territory of electrochemical dilatometry. For instance, quasi 2-dimensional electrode processes like the SEI formation in lithium-ion batteries or the electrochemically driven growth of passivation layers on metal surfaces might become the subject of future dilatometric studies.

The heart of the ECD-3-nano is an electrochemical cell, which is hermetically tight against ambient atmosphere. The two electrodes inside are separated by a stiff glass frit that is fixed in position. The upper (working) electrode is sealed by means of a thin metal membrane through which any charge-induced height change is transmitted towards the sensor/load unit above.

Improvements of the ECD-3-nano (in comparison to previous versions)

  • Elimination of tubing and external valves reduces the risk of leakage and saves effort.

  • Use of special polymer with minimal water absorption reduces drying effort and accelerates work flow.

  • Use of a smaller glass frit reduces amount of electrolyte required (approx. 1 cm³)

  • Better handling saves time and effort.

ECD-3-nano overview

Specifications
Height 230 mm
Width 100 mm
Depth 110 mm
Weight approx. 2.5 kg
Separator diameter 12 mm
Working (upper) electrode diameter 10 mm
Counter (lower) electrode diameter 12 mm
Displacement sensor system capacitive
Displacement range 250 μm
Displacement resolution ≤ 5 nm
Signal drift (sample-free) ≤ 20 nm / hour
Test specimen Electrode films, optional single crystals / grains Diameter ≤ 10 mm, thickness ≤ 1 mm
Load on test specimen approx. 1 N
Chemical compatibility Aprotic organic electrolytes; optional aqueous electrolytes
Cell electrolyte volume approx. 0.5 ml
Temperature resistance -20 to +70 °C (Cell and Sensor)
0 to +40 °C (Conditioning electronics and data logger)
Manuals
Delivery scope
# Component Order no.
1 ECD-3-nano dilatometer, assembled ECD3-00-0001-A
2 Box ECD-3-nano, assembled ECE1-00-0006-F
3 Sensor-GND cable ECE1-00-0041-A
4 Sensor cable (PISeca) SEN9023
5 ECD cell cable ECE1-00-0033-F
6 Power supply SPU 45E-303 ELT9207
7 Power cord IEC 60320 C14 EURO L sw 1.5 m ELT9222
8 USB cable typ A/B (2.0 m) ELT9167

9 Component Order no.
8 USB stick containing EC-Link data logger software ECE1-00-0052-B
10 Allen wrench 2.5 mm WZG9059
11 Allen wrench 3 mm WZG9058
12 3 x PE Seal II ECD-3 piston ECC1-01-0044-D
13 3 x PTFE Seal ECD-3 piston ECC1-00-0044-C
14 1 x PTFE Seal ECD 33.3 x 1.8 mm (3 pcs.) ECC1-01-0043-D/3
15 3 x O-Ring 33 mm x 1.78 mm DIC9034
16 3 x O-Ring 50.5 mm x 1.78 mm DIC9038
17 T-Frit 10/12.5 ECC1-00-0041-B
18 Stiff plate ECD1-00-0041-A
19 3 x Ferrule 1.5 mm (short top part) ECC1-00-0029-H
20 Membrane (aprotic) 1.4404 ECC1-00-0019-D
21 Spacer disc Set 2.1 – 2.3 mm (3 pcs) ECC1-01-0012-F
22 Separator (GF/A) 12 mm x 0.26 mm (10 pcs) ECC1-01-0012-Q/X
23 Demonstration kit for ECD ECD1-00-0900-A
24 Allen wrench set (0.9 / 1.3 / 1.5 / 2) (4 pcs) ECC1-01-0028-A
25 Open end wrench AF7 ECC1-09-2037-A
26 Removing tool for ECD-3 piston ECC1-09-2005-A
27 Allen screw driver 2.5 mm WZG9003
28 Spherical allen screw driver 3 mm WZG9002
29 Tweezer antiacid / stainless WZG9001
Upgrade kits

Upgrade kits for typical configurations

In the standard configuration, the ECD-3-nano is equipped for aprotic electrochemistry (dilatometer cell, sensor and sensor-controller with dc-voltage output -10 to 10 V) with integrated USB data logger. Materials in media contact are stainless steel and PEEK. The user has to provide all peripheral equipment like temperature chamber and potentiostat.

Various add-ons are available for special testing requirements:

Upgrade Kit Aqueous: replaces stainless steel parts by gold parts and thus makes the ECD-3-nano compatible with aqueous electrochemistry.

ECD-3 Full Cell Kit: Part kit for testing full cells without T-frit.

Part Kit for Testing Single Crystals/Grains: Part kit for using single grains or crystals instead of bound electrode films.

Consumables
Cell Body:
T-Frit 10/12.5 (5 pcs.) ECC1-00-0041-B/V
Membrane (aprotic), stainless steel (3 pcs.) ECC1-00-0019-D/3
O-Ring 33.05 mm x 1.78 mm (10 pcs.) DIC9034/X
O-Ring 50.5 mm x 1.78 mm (10 pcs.) DIC9038/X
O-Ring 2.0 mm x 1.0 mm (10 pcs.) DIC9037/X
O-Ring 9.75 mm x 1.78 mm (10 pcs.) DIC9006/X
Ferrule 1.0 (10 pcs.) ECC1-00-0029-B/X
Ferrule 1.5 (10 pcs.) ECC1-00-0029-C/X
PTFE Seal for ECD (33 x 1.8) (3 pcs.) ECC1-01-0043-D/3
PE Seal II for ECD-3 piston (3 pcs.) ECC1-01-0044-D/3
PTFE Seal ECD-3 piston ECC1-01-0044-C/3
PE-Seal (for use with upgrade kit aqueous only) ECC1-01-0044-B/3
Spacer disc (set) 2.1-2.3 ECC1-01-0012-F
Spacer disc (set) 1.8-2.0 ECC1-01-0012-G
Spacer disc (set) 1.5-1.7 ECC1-01-0012-H
Spacer disc (set) 1.2-1.4 ECC1-01-0012-K
Spacer disc (set) 0.9-1.1 ECC1-01-0012-L
Separator (GF/A) 12 x 0.26 mm, (10 pcs) ECC1-01-0012-Q/X
Sealing Set II ECD-3: ECC1-01-0004-E
10x Ferrule 1.5 ECC1-00-0029-H
10x PTFE-Seal for ECD (33.3 x 1.8) ECC1-01-0043-D
10x PTFE Seal ECD-3 piston ECC1-01-0044-C
10x PE Seal II for ECD-3 piston ECC1-01-0044-D
10x O-Ring 33.05 mm x 1.78 mm DIC9034
10x O-Ring 5.0 mm x 1.0 mm (AP370) DIC9036
10x O-Ring 2.0 mm x 1.0 mm DIC9037
10x O-Ring 50.5 mm x 1.78 mm DIC9038
Sensor Unit:
Socket screw DIN-912 M4 x 12
Spare parts

<strong>Sensor unit</strong>

<a href=”https://el-cell.com/wp-content/uploads/2016/03/ECD-3-nano_Spare-parts_sensor-unit.png”><img class=”alignnone wp-image-4213″ src=”https://el-cell.com/wp-content/uploads/2016/03/ECD-3-nano_Spare-parts_sensor-unit.png” alt=”” width=”750″ height=”625″ /></a>

<strong>Cell Body</strong>

<a href=”https://el-cell.com/wp-content/uploads/2016/03/ECD-3_Spare-parts_cell_body.png”><img class=”alignnone wp-image-4206″ src=”https://el-cell.com/wp-content/uploads/2016/03/ECD-3_Spare-parts_cell_body.png” alt=”” width=”750″ height=”625″ /></a>

<strong>Shut-off valve</strong>

<a href=”https://el-cell.com/wp-content/uploads/2016/03/ECD-3_Spare-parts_shut-off-valve.png”><img class=”alignnone wp-image-4208 size-full” src=”https://el-cell.com/wp-content/uploads/2016/03/ECD-3_Spare-parts_shut-off-valve.png” alt=”” width=”1190″ height=”992″ /></a>

<strong>Central CE piston</strong>

<a href=”https://el-cell.com/wp-content/uploads/2016/03/ECD-3_Spare-parts_central-ce-piston.png”><img class=”alignnone wp-image-4209 size-full” src=”https://el-cell.com/wp-content/uploads/2016/03/ECD-3_Spare-parts_central-ce-piston.png” alt=”” width=”1190″ height=”992″ /></a>

<strong>Spring load</strong>

<a href=”https://el-cell.com/wp-content/uploads/2016/03/ECD-3_Spare-parts_spring_load.png”><img class=”alignnone wp-image-4203″ src=”https://el-cell.com/wp-content/uploads/2016/03/ECD-3_Spare-parts_spring_load.png” alt=”” width=”750″ height=”625″ /></a>

<strong>REF electrode ECD, long</strong>

<a href=”https://el-cell.com/wp-content/uploads/2016/03/ECD-3_Spare-parts_ref-electrode.png”><img class=”alignnone wp-image-4202″ src=”https://el-cell.com/wp-content/uploads/2016/03/ECD-3_Spare-parts_ref-electrode.png” alt=”” width=”750″ height=”378″ /></a>

Frequently asked questions
What are the differences between the built-in sensors of the ECD-3 and ECD-3-nano?

The sensors of ECD-3 and ECD-3-nano are both able to detect very small expansions of the electrodes. The main difference between the two devices lies in the detection resolution. The ECD-3 uses an LVDT sensor with a resolution of 50 nanometers with a maximum displacement range of 500 μm. The ECD-3-nano uses a capacitive sensor system with a resolution of 5 nanometers and a maximum displacement range of 250 μm.

Why is it possible to measure displacement values below zero?

The dilatometer does only measure the displacement (=change in thickness), but not the total thickness. The initial displacement reading is arbitrary and can be changed by just turning the micrometer screw at the sensor head. In practice, you turn the micrometer screw so that the initial reading is in the range of zero +/- 20 µm. After the measurement, for convenience, you substract some offset value, so as to set the displacement value exactly to zero at that point in time, where you have started the electrochemical cycle.

How can I clean the T-Frit? How much does a stained T-frit affect future results?

The frit is made of borosilicate 3.3 glass (Duran®) and so can be cleaned with any agents lab glass is compatible with, including e.g. hot aqueous HNO3. According to our experience, the staining of the T-frit does not affect electrochemical results.

Videos

Assembly and disassembly of the ECD-3 and ECD-3-nano electrochemical dilatometer (04/2022)

In this step-by-step video tutorial, Dr. Matthias Hahn guides you through the assembly and disassembly of the ECD-3 and ECD-3-nano electrochemical dilatometer.

UPDATED CONTENT

Assembly of the Full Cell kit for ECD-3 and ECD-3-nano electrochemical dilatometer (03/2022)

In this video, Dr. Matthias Hahn shows you how to assemble the parts of the Full Cell Kit for the ECD-3 dilatometer.

Gallery

Connecting the ECD-3Connecting the ECD-3
Connecting the controller boxConnecting the controller box

Sample test results

Diagrams1

 

Expanding and shrinking of a graphite electrode during lithium insertion and extraction (figure left). The detailed view on the right shows the onset of expansion at 1.9V vs. Li / Li+ (figure right).

 

Current response and height change of layered ruthenium oxide HRO in 2 M H2SO4 during slow scan voltammetry. Courtesy of Prof. Wataru Sugimoto, Shinshu University, Japan.

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