User Manual - EL-CELL
Contents
1. M OF eco 0001 Garg tebe for BCD 3 EL CELL nee 1 R l4 1 X vm rnc tm TTE l 2 owes Nava m f 1 e f EL CELL User Manual ECD 3 Release 1 0 Page 9 of 33 5 Start Up If your are using the ECD 3 the first time please follow the below procedure starting at step 1 After unpacking the ECD 3 remove the Remove the two inner screws first then 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 Release 1 0 Page 10 of 33 EL CELL User Manual ECD 3 Release 1 0 Page 11 of 33 EI CFIBPGC User Manual ECD 3 Release 1 0 Page 12 of 33 Et ann Bee 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 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 Release 1 0 Page 13 of 33 6 Assembling the cell insi2. CC1 00 0019 D O Ring 33 05 x 1 78 mm DIC9005 O Ring 2x 1 5 mm 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 Release 1 0 Page 27 of 33 15 Technical Support Technical 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 neglec
3. EL CELL electrochemical test equipment User Manual Release 1 0 Electrochemical Dilatometer ECD 3 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 Release 1 0 Page 2 of 33 Content 1 Product DescripUlOll i iessceoxchd spp a od CoA RR ASA UAE A dad bis Cl vida Cea MULA RDUM adea 4 AME WU E O O O O O 7 9 Safety 80186651011013 iiid mda olii i end condones dc Pind 8 E i o 4E 8 SS tg tor r E E eer ee 10 6 Assembling the cell inside the glove box eee 14 7 Further assembling outside the glove box eeeeeeeeenne 18 8 EC Link Software Installation eeeeeeeeeennen enn 22 9 C llbration and Settings cies 22 10 Recording the Displacement Signal with an External Potentiostat 23 11 Using the Reference
4. Electrode ccccccceeeeeeeeeeseeeeeeeeeeseeeesgeereganetsaeenes 24 12 Dilatometer Disassembly and Cleaning cccccccceeee 25 13 Core og ce eee 26 I4 CONSUM ADIOS ocasion oss cies totes ee ve toes ces 27 15 Technical Support sese iino ni o ico a eol cc RR Rc D RR c n 28 16 ga en e re er er a rie delet 28 Appendix Components 5811581 rige M M 29 Components Cell BOUNssxcesseaaaebrsetisci qd VES Un dd DEI LEN RUE ITE FU RE NC eN DUCI NEP IPM KE REME 30 Connecter and Cable 0010101 ien PCM IMS ODER LION C ODDDUDDE 31 EL CELL User Manual ECD 3 Release 1 0 Page 3 of 33 1 Product Description The ECD 3 electrochemical dilatometer is dedicated to the measurement of charge induced strain expansion and shrinkage of electrodes down to the nanometer range The ECD 3 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 or 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 ambient atmosphere The two electrodes inside are separated by a stiff glass frit which is fixed in position Th
5. de 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 Attach the T Frit Inside the glove box Put the lithium with 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 O Rings and assemble the dead volume to piston from below the cell base again EL CELL User Manual ECD 3 Release 1 0 Page 14 of 33 User Manual ECD 3 Release 1 0 Page 15 of 33 WZ User Manual ECD 3 Release 1 0 Page 16 of 33 Inside the glove box Lithium must not Inside the glove box Attach the come into contact with the Teflon of the reference pin to the cell body ferrule 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 attaching it to the cell body you can take it outside the glove box EL CELL User Manual ECD 3 Release 1 0 Page 17 of 33 Before fitting the sensor unit on top of the cell body it must be ensured that the sensor tip is in its highest possible position This ensures that the sensor tip is not pressed accidentally through the membrane when screwing on the sensor unit When th
6. e 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 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 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 mps provided on the ECD 3 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 um v with f0 V 125 um max l 1 1 V 29 um m n Analog IN 2 Vi Convert EA om TZT with j0 V 0 C max 10 v 80 C min EL CELL User Manual ECD 3 Release 1 0 Page 23 of 33 11 Using the Reference Electrode The reference electrode assembly is comprised of the reference pin 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 co
7. e sensor tip is pressed through the membrane the sensor unit may be damaged User Manual ECD 3 Release 1 0 Page 18 of 33 E uc d rn cz Now you have to connect all cables as showing in the following photo 1 EDC 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 EL CELL User Manual ECD 3 Release 1 0 Page 19 of 33 a Release the locking screw 1 Then release Adjust the sensor position gap width by the excenter counter clockwise 2 turning the micrometer screw counter clockwise Countersink the sensor tip by turning the micrometer screw counter clockwise Turn the micrometer screw until the flexure will move to the central position The central position of the flexure is also displayed at the LED bar graph indicator at the electronic box of the ECD 3 Turn it until the bar graph indicator at the controller box is approximately in the center position Turn it until the bar graph indicator at the controller box is approximately in the center position EL CELL User Manual ECD 3 Release 1 0 Page 20 of 33 Open the shut off valve in order to connect Example Connecting a Biologic data logger the dead volume with the cell volume cable available on request View the whole wiring on page 19 Finally connect your potentiostat or battery tester to the 4 mm jacks on the front pa
8. e 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 of the working electrode without any interference from that of the counter electrode CE Membrane Current collector REF WE working electrode CE counter electrode Current collector A high resolution displacement LVDT transducer detects dimensional changes of the WE ranging from 100 nanometers up to 500 micrometers during one and the same experiment that may last between 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 For best accuracy and drift stability the dilatometer is to be operated inside a temperature controlled chamber EL CELL User Manual ECD 3 Release 1 0 Page 4 of 33 Basic structure oft the ECD 3 Sensor unit Details shown on the following page Cell body Bracket EL CELL User Manual ECD 3 Release 1 0 Page 5 of 33 Cut drawing oft the ECD 3 Micrometer screw Sensor plunger LVDT sensor NN 1 g Excenter Flexure Load Locking screw Sensor Tip Spacer disc g Glas T Frit in as ri s aay l S Em Shut off va
9. f 33 Components Cell Body Socket screw DIN 912 M4x10 Cover flange ECC1 00 0016 B Membrane aprotic ECCI 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 2 x 1 5 mm DIC9025 EN x 3 gt x 3 gt x ne 2 pea L 7 7 7 7 7 T Frit 10 12 5 ECC1 00 0041 B Shut off valve assembled ECC1 00 0155 B P ot Socket screw DIN 912 M2 5x10 aor 7 ECD 3 base body ECC1 00 0212 A 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 Release 1 0 Page 30 of 33 Connector and Cable Pin out Sensor Cable 5 x 1 x 0 14 mm shielded ECE1 00 0036 A One end of 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 MT Cable Color BEEN EL CELL U
10. llar 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 pin 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 A OF Ferrule 1 5 mm PTFE ECC1 00 lars 0029 C a O Ring 5 x1 mm EPDM DIC9023 ux ie nll Fitting long with cone PPS Techtron 1000 natur ECC1 00 0039 J Reference electrode long 1 4404 ECC1 00 0062 L 77 oo par 77 pud or aan E agii pent P Set collar 1 7 mm 1 4305 d ECC1 00 0038 C uw Set screw M dd DIN 916 M2x2 P d a ae T Compression spring Au 1 4310 FED9017 Hollow screw 1 4305 ECC1 00 0040 A EL CELL User Manual ECD 3 Release 1 0 Page 24 of 33 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 the cell cable from
11. lve Reference electrode 3 Te me Piston EL CELL User Manual ECD 3 Release 1 0 Page 6 of 33 2 Features The ECD 3 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 are briefly described in the following LVDT sensor system with lt 50 nm resolution drift stability of lt 100 nm hour sample free instrument at constant temperature and 500 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 0 3 N or 1 3 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 mm EL CELL User Manual ECD 3 Release 1 0 Page 7 of 33 3 Safety Precautions Use proper safety precautions when using hazardous electrolytes Wear protective glasses and gloves to protect you against electrolyte that
12. 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 company inspection List of Components 1 2 ECD 3 dilatometer ECD3 00 0025 A assembled Box ECD 3 ECE1 00 0006 E assembled ECD sensor cable ECE1 00 0036 A ECD cell cable ECE1 00 0033 E assembled Power supply 15W 24V DC ELT9045 Power supply adapter ELT9078 USB cable typ A B 2 0 m ELT9167 we uml res E EL CELL User Manual ECD 3 Release 1 0 Page 8 of 33 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 EL CERL EC Link Software pe oar o eme w
13. nel of the controller box Make sure that both instruments share a common ground GND potential 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 want we 0 we oe 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 creeping 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 Release 1 0 Page 21 of 33 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 integra
14. ser Manual ECD 3 Release 1 0 Page 31 of 33 Cell Cable 4 x 2 x 0 25 mm TP shielded ECE1 00 0033 E One end of the cable is terminated by a Sub D HD M15 connector to box the other end is terminated by 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 tied to the Sub D connector housing ML Cable Color Color of 2 mm connector EL CELL User Manual ECD 3 Release 1 0 Page 32 of 33 Biologic Auxiliary Cable 2 x 2 x 0 14 mm TP shielded ECE1 00 0039 B One end of the cable is terminated by a Sub D HD F15 connector to the data logger connector at the controller box the other end is terminated by a Sub D M9 connector to 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 EL CELL User Manual ECD 3 Release 1 0 Page 33 of 33
15. t 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 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 Release 1 0 Page 28 of 33 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 Release 1 0 Page 29 o
16. ted 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 controller box Launch the 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 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 txt from the CD into the installation directory of the EC Link software EL CELL User Manual ECD 3 Release 1 0 Page 22 of 33 10 Recording th
17. the dilatometer cell 2 Remove the dilatometer cell from the temperature chamber 3 Detach the sensor load 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 detach the reference electrode In contrast to the initial start up of the dilatometer also the shut off valve must be dismantled after testing see both pictures below Unscrew the socket screw Then remove 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 start at step 15 chapter 6 again EL CELL User Manual ECD 3 Release 1 0 Page 25 of 33 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 Saver Siliconas 4 Take some silicone grease on a sponge or Clean the seals with the silicone grease towel Clean the O Rings with the silicone grease EL CELL User Manual ECD 3 Release 1 0 Page 26 of 33 14 Consumables Cell Body T Frit 10 12 5 ECC1 00 0041 B Membrane aprotic 1 4404 E
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