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User Manual

ECD-3

Release 1.6

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

Содержание ECD-3

Страница 1: ... 2017 EL CELL GmbH 2022 EL Cell GmbH User Manual Release 1 6 Electrochemical dilatometer ECD 3 ...

Страница 2: ... 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 49 40 79012 737 fax 49 40 79012 736 e mail info el cell com web www el cell com ...

Страница 3: ...y 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...

Страница 4: ...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 nano...

Страница 5: ...Page 5 of 47 User Manual ECD 3 Release 1 6 The basic structure of the ECD 3 Sensor unit Details shown on the following page Cell body Bracket ...

Страница 6: ... User Manual ECD 3 Release 1 6 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 ...

Страница 7: ...0 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...

Страница 8: ...ges 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 ECE...

Страница 9: ... 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...

Страница 10: ...llen 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 ...

Страница 11: ...ral 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 1 After unpacking the ECD 3 remove the transport lock from the sensor unit 6 3 Unscrew and detach the sensor unit 6 2 Unscrew the two inner screws first only then the two outer screws ...

Страница 12: ...Page 12 of 47 User Manual ECD 3 Release 1 6 6 4 Screw off the cell body from the bracket 6 5 Unscrew the spring load from the cell body 6 6 Unscrew the reference electrode 6 7 Remove the cover flange ...

Страница 13: ...ate 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 ...

Страница 14: ... 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 ...

Страница 15: ...Page 15 of 47 User Manual ECD 3 Release 1 6 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 ...

Страница 16: ...Page 16 of 47 User Manual ECD 3 Release 1 6 6 17 Remove the socket screw at the end of the piston and disassemble it Both seals need to be renewed before each test ...

Страница 17: ... 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 ...

Страница 18: ...s 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 ...

Страница 19: ... 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...

Страница 20: ...7 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 ...

Страница 21: ...glove box Tighten the socket screw at the end of the piston firmly using the tools provided Important note Only use a frit flange with an attached metal support ring as shown in the picture Otherwise the frit flange may be damaged when trying to tighten the screw 7 9 Inside the glove box Put this assembly into the cell base body Make sure that the two grooves at the frit flange and the cell base b...

Страница 22: ...the glove box Add 320 420 μl of electrolyte using an pipette 7 11 Inside the glove box Place the working electrode with the active side pointing downwards on top of the T Frit 7 12 Inside the glove box Insert the PTFE seal make sure it is inserted correctly ...

Страница 23: ...ove box Then put the membrane on top 7 15 Inside the glove box Hold the pushbutton on the reference pin pressed and pick up some lithium with the reference pin Make sure that the hole of the reference pin is completely filled with lithium metal Incomplete filling may result in scatter noise of the WE potential Make sure that the reference pin and the PTFE ferrule are not corroded or damaged The PT...

Страница 24: ...pin gently to the cell body Push onto the back of the reference pin while screwing it in 7 17 Inside the glove box Attach the cover flange 7 18 Inside the glove box Now close the cell body with the three cover screws In the first step tighten the screws slightly with the enclosed screwdriver ...

Страница 25: ...mend using the allen key to tighten the screws in small increments on all three sides until they reach the stop 7 20 Inside the glove box Then check that the cell cover is firmly seated on the housing and that no gap is visible 7 21 Inside the glove box Now tighten the reference pin firmly ...

Страница 26: ...ser Manual ECD 3 Release 1 6 7 22 Inside the glove box Now screw in the spring load into the cell base 7 25 Inside the glove box The cell is now assembled and hermetically sealed and can be removed from the glove box ...

Страница 27: ...2 Unlock the locking screw 1 and the excenter 2 Then turn the micrometer screw 3 clockwise until the sensor tip is in the upmost position Note Not following the above instruction may result in damage of the membrane the glass frit or even the sensor unit when attaching the sensor unit onto the dilatometer cell 3 2 1 8 3 Attach the sensor unit onto the dilatometer cell ...

Страница 28: ... We highly recommend operating the dilatometer in a temperature controlled environment 1 ECD 3 cell cable 2 ECD sensor cable 3 Power supply power supply adapter 4 USB cable 5 Example Individual Biologic data logger cable available on request 8 4 Fasten the screws to fix the sensor unit 4 2 3 1 5 ...

Страница 29: ...r at the electronic box of the ECD 3 Any yellow LED indicates a valid position For best accuracy and resolution adjust the sensor approximately in central position 8 5 Unlock the locking screw 1 and the excenter 2 if not already done 2 1 8 6 Lower the sensor tip by turning the micrometer screw counter clockwise ...

Страница 30: ...or open circuit for several hours to allow for baseline stabilization The initial rest period helps discern charging induced dimensional changes from the initial creeping NOTE All materials display a more or less pronounced creeping They tend to shrink when applying a load and swell when removing it A significant contribution to the initial creeping seen right after cell assembly is to be assigned...

Страница 31: ...nnection and you are ready to start the measurement Additional information on the EC Link software can be found in a separate manual https el cell com support manuals 10 Calibration and Settings Calibration of the instrument has been carried out at the factory The corresponding settings of the EC Link software are stored in the file Settings V2 in the installation directory on the local hard drive...

Страница 32: ... the analog input of the respective VMP3 channel 2 In the Biologic EC Lab software load the experiment settings ECD mps provided on the ECD 3 installation media The settings are shown in the External Devices dialog Adapt the Parameter Settings of the charge discharge protocol to your particular experiment if necessary ...

Страница 33: ...nto the back of the reference pin while screwing in the pin NOTES Avoid any direct contact of the PTFE ferrule with lithium metal PTFE is being reduced to black and porous carbon when getting in contact with lithium Renew the PTFE ferrule after each experiment The standard dilatometer comes with a stainless steel reference pin which is good for use with lithium metal In contrast the gold reference...

Страница 34: ...a specialized frit flange When running the experiment the valve should be open This way unwanted pressure build up via gas evolution is effectively mitigated NOTES Close the valve gently by hand Excessive torque may damage the valve Some valve parts may get into electrolyte contact Therefore it is advised to unscrew the valve seating and stem after use The two O ring seals and the PTFE ferrule may...

Страница 35: ... current collector and the working electrode Choose a proper spacer disc height depending on the thickness of your electrode Spacer discs are available in different heights ranging from 0 9 mm to 2 7 mm in 0 1 mm steps for a complete list see page 37 If in doubt choose the next higher spacer disc We recommend using the 2 7 mm spacer disc for all electrodes in the thickness range of 0 to 150 µm Sen...

Страница 36: ...he dilatometer cell and the sensor unit 2 Remove the dilatometer cell from the temperature chamber Then follow the instructions described in chapter 6 starting at step 3 Clean all wetted parts right after disassembly Ultrasonic cleaning with water and or detergent wash is recommended Valves and tubing may clog if not purged adequately with water or another solvent After cleaning dry all parts at 8...

Страница 37: ...10 pcs DIC9034 X Ferrule 1 0 10 pcs ECC1 00 0029 B X Ferrule 1 5 10 pcs ECC1 00 0029 H X O Ring 50 5 x 1 78 mm 10 pcs DIC9038 X PTFE seal for ECD 33 x 1 6 3 pcs ECC1 01 0043 D 3 PTFE seal for ECD 3 piston 3 pcs ECC1 01 0044 C 3 Spacer disc set 2 1 2 7 ECC1 01 0374 A 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 ...

Страница 38: ...ge 38 of 47 User Manual ECD 3 Release 1 6 18 Spare Parts Components Sensor Unit There are no further spare parts available for the sensor unit For repair please contact EL CELL Socket screw DIN 912 M4x12 ...

Страница 39: ...Page 39 of 47 User Manual ECD 3 Release 1 6 Components Cell Body ECD3 00 0002 A ...

Страница 40: ... Manual ECD 3 Release 1 6 Shut off valve ECD 3 assy ECC1 00 0155 B Ferrule plug 1 0 ECC1 00 0029 B O Ring 5x1 mm AP370 DIC9036 O Ring 2x1 mm AP312 DIC9037 Valve Seating ECD 3 ECC1 00 0153 C Valve Stem ECD ECC1 00 0063 B ...

Страница 41: ...Page 41 of 47 User Manual ECD 3 Release 1 6 Central CE piston ECD 3 PE sealed screwed ECD3 00 0006 D ...

Страница 42: ...elease 1 6 Spring load ECD 3 assy ECD3 00 0008 A Compression Spring 1 2 x 9 8 x 19 2 x 3 5 AU FED9021 Spring Ram ECD 3 ECC1 00 0022 E O Ring 6 75 x 1 78 mm AP380 DIC9039 O Ring 14 x 1 5 mm AP370 DIC9032 Spring Ram ECD 3 ECC1 00 0021 C ...

Страница 43: ...long assy 1 4404 ECD1 00 0009 D Ferrule 1 5 short top part ECC1 00 0029 H Fitting long II with cone ECC1 00 0039 N Ref pin ECD long 1 4404 ECD1 00 0050 A Compression spring 1 4310 Au FED9017 Reference connection tip ECC1 00 0331 A Hollow screw ECD 3 ECC1 00 0040 A ...

Страница 44: ...f the cable is terminated by a SUB D F15 connector to box the other end is terminated by a round Binder series 712 connector to LVDT sensor The cable shield is tied to both connector housings Sub D F15 Pin Series 712 Pin Signal Cable Color 1 1 Secondary White 2 2 Secondary Brown 3 5 Secondary Mid Grey 4 5 4 Primary Blue 6 3 Primary Black ...

Страница 45: ...a connectors terminate the other end A Pt100 sensor is located beneath the black shrink tube at the end of the cable pointing to the dilatometer The cable shield is tied to the Sub D connector housing Pin Signal Cable Color Color of 2 mm connector 1 V1 Red Red 2 V2 Blue Blue 3 4 REF Grey Grey 5 I2 Yellow Yellow 6 7 8 9 10 I2 Green Green 11 Pt100 1 Brown 12 Pt100 2 White 13 14 15 ...

Страница 46: ...oller box the other end is terminated by a Sub D M9 connector to the auxiliary input connector of the Biologic potentiostat The cable shield is tied to both connector housings Sub D HD F15 to box Sub D M9 to Biologic AUX Input Pin Signal Cable Color Pin Signal Comments 1 2 3 4 5 6 7 8 9 10 GND Brown 7 GND 11 12 13 Temperature Green 6 Analog IN 2 10 10V 200 C V 14 15 Displacement White 1 Analog IN ...

Страница 47: ...rranty 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 ...

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