User Manual - EL-CELL
Contents
1. 7 ne a BE ae e 1 ne e T Frit 10 12 5 ECC1 00 0041 B Shut off valve assembled ECC1 00 0155 B e E E E ra z oo E A E ra ea a E E E Pa 2 Socket screw DIN 912 M2 5x10 7 ECD 3 base body ECC1 00 0212 A i O Ring 50 5 x 1 78 mm Reference electrode DIC9026 long assembled ECC1 00 0009 D O Ring 33 05 x 1 78 mm DIC9005 Dead volume cover ECC1 00 0211 A Socket screw DIN 912 M4x10 O Ring 9 75 x 1 78 mm DIC9006 Piston ECC1 00 0126 B Spring load assembled ECD3 00 0008 A EL CELL User Manual ECD 3 nano Release 1 0 Page 30 of 32 Connector and Cable Pin out Cell Cable 4 x 2 x 0 25 mm TP shielded ECE1 00 0033 E One end of the cable is terminated with a Sub D HD M15 connector to box the other end is terminated with 2 mm banana connectors A Pt100 sensor is located beneath the black shrink tube at the end of the cable pointing to the dilatometer The cable shield is connected to GND aus Signa Cable Color Color of 2 mm connector EL CELL User Manual ECD 3 nano Release 1 0 Page 31 of 32 Biologic Auxiliary Cable 2 x 2 x 0 14 mm TP shielded ECE1 00 0039 B Both connector housings are tied to the cable shield The cable shield is connected to GND IEEE 1394 to Box Sub D2. 8 eee EE 28 Appendix Componente SNS Or UNIT sersan aranan AAA A 29 COMpOnentS Cell BOG renra 30 Connector ANG Cable EE ee 31 EL CELL User Manual ECD 3 nano Release 1 0 Page 3 of 32 1 Product Description The ECD 3 nano electrochemical dilatometer is dedicated to the measurement of charge induced strain expansion and shrinkage of electrodes down to the nanometer range The ECD 3 nano has been particularly developed for the investigation of Li ion 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 used can either be 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 nano is an electrochemical cell hermetically sealed against ambient atmosphere The two electrodes inside are separated by a stiff glass frit which is fixed in position The upper working electrode WE is sealed by means of a thin metal foil through which any charge induced thickness change is transmitted towards the sensor load unit above This working principle allows determining the height change es Load Membrane Current collector REF WE working electrode CE counter electrode Current collector of the working electrode without any interference from that of the counter electrode CE A high resolution capacitive di
3. EL CEEL electrochemical test equipment User Manual Release 1 0 Electrochemical Dilatometer ECD 3 nano 20 May 2015 2015 EL CELL GmbH 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 49 0 40 790 12 733 fax 49 0 40 790 12 736 e mail info el cell com web www el cell com EL CELL User Manual ECD 3 nano Release 1 0 Page 2 of 32 Content 1 Product DESGCFIDUIOW EE 4 2 FO QU NN 7 3 Safety EEGENEM 8 VC BE 8 oe CH e te 0 2 GEET 10 6 Assembling the cell inside the glove box 14 7 Further assembling outside the glove box 18 8 EtetunkZSottotare tnstoailarteg zageegeeeeeggeegee EES 22 9 Sole heey ee arate os a ee tere eer 22 10 Recording the Displacement Signal with an External Potentiostat 23 11 Using the Reference Electrode cccc ccc cece cence sees ee eeeeaeeeaeeeaeeeaeeeaaeeas 24 12 Dilatometer Disassembly and Cleaning cece esses eeaeeeaeeeeaeeeaeeeaaenes 25 13 e ols 0 E 26 14 CONES aS asc aise strc cso sss esse sees ccs tsetse vines eee 27 15 Technical Support d 2
4. M9 to Biologic AUX Input Displacement Green Analog IN1 EL CELL User Manual ECD 3 nano Release 1 0 Page 32 of 32
5. VMP series is described as an example The Biologic potentiostats feature two analog inputs that are used here to record both displacement and temperature 1 Connect the 9 pin Sub D connector of the optional analog output cable to the analog input of the respective VMP3 channel 2 Inthe Biologic EC Lab software load the experiment settings ECD 3 nano mps provided on the ECD 3 nano documentation CD The settings are shown in the External Devices dialog see screenshot below actual settings may differ Adapt the Parameter Settings of the charge discharge protocol to your particular experiment if necessary Analog IN 1 V Convert EA to Displacement pum e wth oO Ms 1425 um max SE oe um min Analog IN 2 J Convert EA to T C v wth 9 Ve go Cima 10 y 80 C min EL CELL User Manual ECD 3 nano Release 1 0 Page 23 of 32 11 Using the Reference Electrode The reference electrode assembly is comprised of the reference electrode the set collar attached to the pin by means of a set screw the fitting the spring and the hollow screw cf the sketch below The hollow screw serves to apply the spring pressure on the set collar thereby gently pushing the reference pin against the glass frit The blind bore on the tip of the reference pin is intended for taking up the reference electrode material For most lithium ion chemistries the reference material may be a small piece of lithium metal picked up by the reference p
6. any inspection List of Components 1 ECD 3 nano dilatometer ECD3 00 0026 A assembled 2 Box ECD 3 nano ECE1 00 0006 F assembled 3 Sensor GND cable ECE1 00 0041 A 4 Sensor cable PISeca SEN9023 5 ECD cell cable ECE1 00 0033 E 6 Power supply SPU 45E 303 ELT9207 7 Cable connector NC5FRX 5 pole female ELT9207 8 USB cable typ A B 2 0 m ELT9167 Ki Ki EL CELL User Manual ECD 3 nano Release 1 0 Page 8 of 32 Accessories Kit ECD3 00 0400 A 1 2 10 11 12 13 14 4 x O Ring 33 05 mm x 1 78 mm DIC9005 2 x O Ring 9 75 mm x 1 78 mm DIC9006 2 x O Ring 2 mm x 1 5 mm DIC9025 2 x O Ring 50 5 mm x 1 78 mm DIC9026 Membrane aprotic 1 4404 ECC1 00 0019 D Spacer disc set 2 1 2 3 ECC1 01 0012 F Demonstration kit 5 x activated carbon electrode foil w 5 PTFE Binder 10 mm ECD1 00 0900 A Filling tube ECD3 01 0001 A CD containing EC Link data logger software ECE1 00 0052 A Tweezers WZG9001 Spherical allen screw driver 3 mm WZG9002 Allen screw driver 2 5 mm WZG9003 Vacuum tweezers WZG9004 Set allen wrench ECC1 01 0028 A EC Link software gt _ aa EL CELL l EL CELL OG o OCG 2 pa J DRAS x 1 78 ah _ Mali gaer e p SC WW Wm Tt EL CELL Date ring 9 75 w3 e 2 EL CELL A ECD3 D1 0001 A filing tube for ECD 3 Lo EL CELL User Manual ECD 3 nano Release 1 0 Page 9 of 32 5 Start Up If your are using the ECD 3 nano th
7. attaching it to the cell body you can take it outside the glove box EL CELL User Manual ECD 3 nano Release 1 0 Page 17 of 32 User Manual ECD 3 nano Release 1 0 Page 18 of 32 Now connect all cables as shown in the pictures 1 ECD cell cable 2 Sensor GND cable 3 Sensor cable 4 Power cord 90 to 240V AC input 5 DC cable 15V 15V 5V DC output 6 USB 2 0 cable 7 Optional analog output cable EL CELL User Manual ECD 3 nano Release 1 0 Page 19 of 32 EL CELL f EL CELL Open the shut off valve in order to connect Example showing the connection of a the dead volume with the cell volume This Biologic potentiostat to the controller box minimizes the build up of gas pressure during the cycle experiment Finally connect your potentiostat or battery tester to the 4 mm jacks 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 http www bio logic info electrochemistry ec lab instruments Controller Box Potentiostat Biologic Potentiostat VSP VMP3 etc ee ee ee sets ae Before starting the electrochemical cycle we recommend holding the cell at constant potential or open circuit for several hours to allow for baseline stabilization The initial rest period helps to discern charging induced dimensional changes from the initial creepin
8. chnical support for this product is exclusively provided by EL CELL GmbH EL CELL GmbH Tempowerkring 8 21079 Hamburg Germany phone 49 0 40 790 12 733 fax 49 0 40 790 12 736 e mail info el cell com web www el cell com 16 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 t
9. detach the reference electrode In contrast to the initial start up of the dilatometer also the shut off valve must be disassembled after testing SZ Important Dissassemble and clean the shut off valve Clean all wetted parts right after disassembly Ultrasonic cleaning with water and or detergent wash is recommended Valves and tubing may clog if not properly purged with water or other solvent After cleaning dry all parts in vacuum at 80 C overnight For further tests follow the instructions beginning at step 15 chapter 6 EL CELL User Manual ECD 3 nano Release 1 0 Page 25 of 32 13 Care Instructions Maintain the O Rings regularly with silicone grease We recommend to use new O Rings for each measurement in order to achieve best results Wipe the seal at the valve stem with the sponge Take some tiny amount of silicone grease on a sponge or cloth and wipe the O ring seals EL CELL User Manual ECD 3 nano Release 1 0 Page 26 of 32 14 Consumables Cell Body T Frit 10 12 5 ECC1 00 0041 B Membrane aprotic 1 4404 ECC1 00 0019 D O Ring 33 05 x 1 78 mm DIC9005 O Ring 2x 1 5mm DIC9025 O Ring 50 5 x 1 78 mm DIC9026 O Ring 9 75 x 1 78 mm DIC9006 Accessories kit ECD 3 ECD 3 00 0400 A Sensor Unit Socket screw DIN 912 M4 x 12 EL CELL User Manual ECD 3 nano Release 1 0 Page 27 of 32 15 Technical Support Te
10. e first time please follow the below procedure starting at step 1 After unpacking the ECD 3 nano remove Remove the two inner screws first then the the transport lock from the sensor unit two outer screws After that screw off the sensor unit from the bracket Screw off the cell body from the bracket Now unscrew the spring load from the bottom of the cell body EL CELL User Manual ECD 3 nano Release 1 0 Page 10 of 32 User Manual ECD 3 nano Release 1 0 Page 11 of 32 EI EL CELL User Manual ECD 3 nano Release 1 0 Page 12 of 32 km ke ad E ss be All the below shown parts need to be dried before they can be moved into the glove box for assembly Recommended drying conditions 80 C lt 0 01 mbar 12 hours 1 Membrane aprotic 1 4404 2 Spacer disc height depends on the height of your electrode 3 T Frit 4 Cover 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 11 O Ring 50 5 x 1 78 mm 12 2 x O Ring 33 05 x 1 78 mm 13 O Ring 2 x 1 5 mm EL CELL User Manual ECD 3 nano Release 1 0 Page 13 of 32 6 Assembling 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 Inside the glove box Insert the T frit Inside the glove box Put the lithium wi
11. g NOTE All materials display a more or less pronounced creeping They tend to shrink when applying a load and to swell when removing this load A mayor contribution to the initial creeping seen right after cell assembly is to be assigned to the construction materials of the dilatometer Creeping of the working electrode is induced each time the mechanical properties of the working electrode are altered by charging Therefore each charge induced height change is followed by some creeping The charge induced creeping effects are real and not artefacts of the measurement EL CELL User Manual ECD 3 nano Release 1 0 Page 21 of 32 8 EC Link Software Installation In order to record the displacement signal together with the cell voltage cell current electrode potential and temperature the software of the integrated data logger needs to be installed on a Windows PC You must be logged into an account with Administrator privileges Save your work and close down all active programs On the installation CD run X Driver_CDM20814 Setup where X refers to the CD drive This will install the FTDI driver required to establish the USB connection with the data logger On the installation CD run X setup This will install the data logger software Follow any instructions that may appear on your screen Once installation is finished plug in the provided USB cable into both the host PC and the ECD 3 nano controller box Launch t
12. he data logger software if not already done 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 a separate manual http el cell com downloads downloads manuals 9 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 ECD nano 3 Device ID txt in the installation directory on the local hard drive and on the installation CD If the default settings have been changed for any reason the original settings can be restored by copying Settings ECD nano 3 Device ID txt from the installation CD into the directory C ProgramData EC LINK The settings affect only the data logger readings The DIP switches at the controller box affect both the displacement readings of the USB data logger and the analog output signal Leave the switches in their default position as shown in the screenshot below EL CELL User Manual ECD 3 nano Release 1 0 Page 22 of 32 10 Recording the Displacement Signal with an External Potentiostat Many of today s battery testers and potentiostats provide additional analog inputs that may be used to record sensor signals along with cell current and potential In the following the combination of the ECD 3 nano with a Biologic potentiostat MPG 2 SP VSP and
13. he 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 EL CELL User Manual ECD 3 nano Release 1 0 Page 28 of 32 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 EL CELL User Manual ECD 3 nano Release 1 0 Page 29 of 32 Components Cell Body Socket screw DIN 912 M4x10 Cover flange ECC1 00 0016 B Membrane aprotic ECC1 00 0019 D O Ring 33 05 x 1 78 mm DIC9005 Frit flange ECC1 00 0213 A Spacer disc ECC1 00 0018 x O Ring 2x 1 5 mm DIC9025
14. in For other aprotic electrolytes and also for some aqueous systems a piece of PTFE bound activated carbon may serve as the pseudo reference material The optional gold reference pin is recommended for use in aqueous electrolytes NOTE Do not use the gold reference pin in combination with lithium metal as the reference material Components of the reference electrode Ferrule 1 5 mm PTFE ECC1 00 0029 C O Ring 5 x1 mm EPDM DIC9023 Fitting long with cone PPS Techtron 1000 natur ECC1 00 0039 J Reference electrode long 1 4404 ECC1 00 0062 L Ps Set collar 1 7 mm 1 4305 ee ECC1 00 0038 C To Set screw DIN 916 M 2x 2 o e e a e o ei ei a ei N eg ei Se Compression spring Au 1 4310 FED9017 Hollow screw 1 4305 ECC1 00 0040 A EL CELL User Manual ECD 3 nano Release 1 0 Page 24 of 32 12 Dilatometer Disassembly and Cleaning When disassembling the dilatometer cell wear protective gloves and glasses Collect parts that have been in contact with electrolyte on a separate tray for subsequent cleaning 1 Disconnect all cables from the dilatometer cell and the sensor unit 2 Remove the dilatometer cell from the temperature chamber 3 Detach the sensor unit from the dilatometer cell 4 Detach the cell from the bracket Then disassemble the cell body as described in chapter 5 starting at step 4 It is very important to unscrew the spring load first After unscrewing the spring load you can
15. ity of lt 20 nm hour sample free instrument at constant temperature and 250 um full range Conditioning electronics with analog output signals 10 to 10 V for displacement and temperature Integrated USB data logger for the recording of displacement temperature cell potentials and current 3 electrode electrochemical cell Sample working electrode bound electrode film or single crystal grain max sample size 10 mm x 1 mm diameter x thickness Load on working electrode approx 1 N Electrolyte volume approx 1 ml Materials in contact with electrolyte PEEK borosilicate glass EPDM rubber stainless steel 316L for aprotic gold for aqueous electrolytes Operating temperature range Cell and sensor 20 to 70 C Conditioning electronics and data logger 0 to 40 C Dimensions of the ECD 3 nano mm 110 EL CELL User Manual ECD 3 nano Release 1 0 Page 7 of 32 3 Safety Precautions Use proper safety precautions when using hazardous electrolytes Wear protective glasses and gloves to protect you against electrolyte that may accidentally spill out of the instrument during filling operation and disassembly 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 comp
16. splacement transducer detects dimensional changes of the WE ranging from a few nanometers up to 250 micrometers during one and the same experiment that may last between a few minutes to many days The ECD 3 nano 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 For best accuracy and drift stability the dilatometer is to be operated inside a temperature controlled chamber EL CELL User Manual ECD 3 nano Release 1 0 Page 4 of 32 Basic structure of the ECD 3 nano Sensor unit Details shown on the following page Cell body Bracket EL CELL User Manual ECD 3 nano Release 1 0 Page 5 of 32 Cut drawing of the ECD 3 nano Sensor cable Capacitive sensor KE E a Micrometer screw Sensor plunger A A 4 Bai d rer T T AT GE Locking screw Flexure Load Sensor Tip Spacer disc Glass T Frit Shut off valve Reference electrode Piston EL CELL User Manual ECD 3 nano Release 1 0 Page 6 of 32 2 Features The ECD 3 nano is an electrochemical dilatometer for measuring changes of thickness of the working electrode of a battery test cell The main features of the ECD 3 nano are briefly described in the following High resolution capacitive sensor system with lt 5 nm resolution drift stabil
17. th the smaller side pointing downwards counter electrode 10 mm diameter on top into the frit flange of the T frit into the frit flange Inside the glove box Attach the counter Inside the glove box Insert the two big piston from below O rings and assemble the dead volume to the cell base again EL CELL User Manual ECD 3 nano Release 1 0 Page 14 of 32 Inside the glove box Put this assembly Inside the glove box Insert the O ring into the cell base body Make sure to have seal DIC9005 see arrow Then place the the two grooves properly aligned Don t working electrode with the active side down forget to insert the little O Ring seal on top of the T Frit Inside the glove box Put one of the Inside the glove box Then put the provided spacer discs on top of the membrane on top electrode Use the 2 3 mm thick spacer disc for samples of lt 100 um thickness Inside the glove box Attach the cover Inside the glove box Close the cell body flange by tightening the three screws EL CELL User Manual ECD 3 nano Release 1 0 Page 15 of 32 FL CELL User Manual ECD 3 nano Release 1 0 Page 16 of 32 Inside the glove box Lithium must not Inside the glove box Attach the come into contact with the PTFE ferrule reference pin to the cell body see arrow Inside the glove box Make also sure that Inside the glove box The cell is now there is no lithium outside the pin before assembled and hermetically sealed so that
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