User Manual - EL-CELL
Contents
1. EL CELL Valve Support III assy part ECD1 00 0004 D Cap Nut M4 part N_1587 Thread Rod M4 part ECC1 00 0052 B Female Luer to 14 28 Male pa LABOOO6 Shut Off Valve 1 4 28 yellow part LABOO11 Valve Support nano part ECC1 00 0035 D Einwegspritze 5ml part LABOOOS Spacer 4x6x3 Ferrule flangeless 1 32 in 015 part ECC1 00 0050 B part LABO Nut SF short part ECC1 00 0145 A Ferrule flangeless 1 32 in part LABOO15 Shut Off Valve 1 4 28 red part LABOO10 Nut SF short part ECC1 00 0145 A be Cap Nut M4 part N_1587 Ferrule flangeless 1 32 in part LAB0015 EL CELL Page 27 of 34 Sensor unit part ECD2 00 0030 A Page 28 of 34 ECD 2_manual 27 02 2015 Central CE Piston IT aprotic part ECD1 00 0005 B O Ring 9 75x1 78 O Ring 9 75x1 78 part DIC9006 part DIC9006 CE Piston II aprotic part ECC1 00 0020 D Central CE Piston II aqueous part ECD1 00 0006 B CE Piston II aqueous part ECC1 00 0020 C cae A oe Feed Wire part ECC1 00 0032 B Thrust Screw part ECC1 00 0066 A O Ring 9 75x1 78 Ferrule flangeless 1 32 in part DIC9006 part LABOOO7 Page 29 of 34 EL CELL CE Spring Load II part ECD1 00 0008 B Spring 1 0x10x26 Spring Ram I part FED9015 part ECC1 00 0022 C O Ring 15 6x1 78 Adjusting Screw part DIC9008 part ECC1 00 0021 B Reference Electrode aprotic PTFE ferrule part ECD2. 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 oF N SY e 9 ECD 2 DL dilatometer in the assembled state equipped for use with aprotic electrolytes Signal conditioning electronics controller box with integrated USB data logger for recording the displacement temperature cell potentials and current USB data acquisition software Windows drivers and operating manual on CD Cell cable connects dilatometer cell with controller box Sensor Cable connects dilatometer sensor unit with controller box 3 tubing assemblies for interconnection between cell valves and syringe 20 ml syringe for filling the dilatometer cell with electrolyte Vacuum pipette and tweezers for electrode handling Hex wrenches for assembly and maintenance Activated carbon electrodes 5 pcs for reference measurements Page 7 of 34 EL CELL 5 Dilatometer Assembly The following photographs refer to the use of the dilatometer with aqueous electrolytes For aprotic organic electrolytes the assembly differs slightly as indicated in the respective figure captions 1 Insert o rings into cell body 21 95 x 1 78 and 41 x 1 78 Insert glass frit T frit 10 20 mm dia into cell body Page 8 of 34 EL CELL Page 9 of 34 3 Place CE dia lt 20 mm with the active layer downside on top of t
3. stiff glass frit that is fixed in position The upper working electrode WE is sealed by means of a thin metal foil through which any charge induced height 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 LVDT sensor membrane fe REF 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 2 DL 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 Page 4 of 34 EL CELL Sensor plunger Spacer disc for Friction free flexure guide height adjustment Weight load on WE not exchangeable LA oder INS Tuz Je mei Valve assembly for vacuum filling via syringe Metal membrane Auxiliary port Reference electrode Glas T frit assembly Separates WE test Specimen on top from CE below Gas filled dead Volume to suppress changes in hydrostatic l pressure inside cell Spring load
4. 1 00 0009 C Reference Electrode II aprotic part ECD1 00 0009 B Ref Electrode Fitting 1 7mm with cone part ECC1 00 0062 D part ECC1 00 0039 F Reference Electrode II cp iian part ECC1 00 0062 C Ferrule 1 5 part ECC1 00 0029 C Set Screw M2x2 part N_916 Sprin l a A 1 Ys Set Collar 1 7 YX part ECC1 00 0038 C Hollow Screw part ECC1 00 0040 A 14 Connector and Cable Pin out Cell Cable 4 x 2 x 0 25 mm TP shielded Part 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 Color of 2mm Pin Signal Cable Color Connector 1 Red Red 3 e 6 AUX Pink Black e ee ae ee eee Gk a l aooe n 11 Pioo Brown 12 Poo White A e ee Sensor Cable 5 x 1 x 0 14 mm shielded Part 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 Series 712 Pin Pin Signal Color pt 1 Secondary White 2 2 Secondary Brown oa ee o S o 6 3 Primay Black Page 31 o
5. 70 C Connect the Pun connector of the sensor cable to the LVDT sensor Turn on the sensor electronics by connecting the controller box to the 24 V power supply Connect the 2 mm banana plugs of the cell cable to the dilatometer cell Sensor Cable Cell Cable Controller Power Supply T Chamber EL CELL Adjust the sensor target by turning the micrometer screw counter clockwise until the bar graph indicator at the controller box is approximately in mid position tr HEIGHT Page 18 of 34 EL CELL 27 N Fasten the carriae Finally connect your potentiostat or battery tester to the 4 mm jacks on the front panel 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 Controller Biologic Potentiostat Box Potentiostat E MP etc WE Current AY N a CE 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 that all materials display a more or less pronounced creeping They tend to shrink when applying a load an
6. Dilatometer DISASSEMDIY ccsecvescsecusecuecusecuecusecuscuseeueausecueausesueausesueausesues 22 Using the Reference Electrode cccccscseceesecceseeeeeeeeeeeeeeseeeeeeeeeeaeeeeaesesenees 23 Using an Auxiliary Electrode cccscsecscseceeeeceseeeesseeeeeeeeeaeeseeeetaesesaesesanees 23 Using Single Crystals or Grains as the Working Electrode option 08 24 SAS IU es aE nteaenione tne oanie EEE alee enero neve A ARA 26 Connector and Cable Pin OUt cccccceeeceeeeeeeeeeeeeeaeea esa eea esa eeaeeaeeaeeeeaeeaees 31 TeCHIMIGAl SUDDOUE sis scrnsneeniiensssuaoseeniiesstouenasnenseannaneeanieasindasunaiaee niente 33 wWairanty perenne a aa a A 34 Page 3 of 34 EL CELL 1 Product Description The ECD 2 DL electrochemical dilatometer is dedicated to the measurement of charge induced strain expansion and shrinkage of electrodes down to the sub micrometer range The ECD 2 DL 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 organic as well as aqueous electrolyte solutions The electrode materials used can either be bound film or single crystals grains e g HOPG or graphite flakes The maximum sample size is 10 mm x 1 mm diameter x thickness The heart of the ECD 2 DL is an electrochemical cell hermetically sealed against ambient atmosphere The two electrodes inside are separated by a
7. EL CELL electrochemical test equipment Electrochemical Dilatometer ECD 2 DL User Manual Release 1 8 EL Cell GmbH PCB ECD 2 DL 8 2 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 D 21079 Hamburg Germany phone 49 0 40 790 12 733 fax 49 0 40 790 12 736 e mail info el cell com web http el cell com Page 2 of 34 EL CELL Contents O N AW WO A U N e e e e e e e e O a BR U N e O Product DESCHIDUION oirir noon E 4 Technical Specifications ccccecsececcecveueuseeeeceaveueuseueeuvaveueuseueeavaveueuneueeavarenss 5 Safety PrecautionS s sssssssunnnnannnnnnnnnnnnannnnnnnnnnnnannnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnn 6 Bosen a E PE E E E EE EE E A E 7 Dilatometer Assembly cceadisacssstintarsndivessandvatedseddseinenaneindssdeatsxsedindsesbretewesdets 8 EC LINK Software Installation cccccscceeseesessceeeceeceseeceseeoesesceeseeaeceeoes 20 Settings and Calibration ccccscsecscceceececseceeeeseeeesecseseeaeseecuseesesaeeesaeeesanees 20 Recording the Displacement Signal with an External Potentiostat 21
8. art the measurement Additional information on the EC LINK software can be found in the EC LINK Quick Start Guide 7 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 8 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 2 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 displacement and temperature 1 Device Type Device Name ECD 2 DL E Dilatometer Analog OUT Convert to EN with la E W max D D VW mir Analog IN 1 M Convert E to Displacement um Y with 3702 ES z j um mas t 7300 pm rear Analog IN M Convert Ey with fD 0 C max f 0 ie E C min Page 21 of 34 Connect the 9 pin Sub D connector of the optional a
9. d copper 3 pieces ECC1 00 0019 F Membrane cranked aluminium 3 pieces Page 25 of 34 EL CELL 13 Spare Parts Socket Screw M4x30 part N_912 i oe Cover Flange part ECC1 00 0016 B gt Socket Screw M4x25 part N_912 Say spacer disc S part ECC1 00 0018 A part ECC1 00 0018 C _ part ECC1i 00 0018 D part ECC1 00 0018 E Ferrule plug part ECC1 00 0029 D Nut part ECC1 00 0125 A Cell Body a part ECC1 00 0015 C Ring f part LAB0015 kacs a Nut SF short a part ECC1 00 0145 A PA Co Ferrule flangeless 1 32in part LABOO15 Cell Bottom Cell II assy part ECD1 00 0002 D Membran a part ECC1 00 0019 A Nut SF short part ECC1 00 0145 A _Ferrule ae 1 32 in _ part LABOO15 O Ring 33 05x1 78 part DIC9005 T Frit part ECC1 00 0041 A Kontaktscheibe part ECC1 00 0033 A part ECC1 00 0011 B_ Central CE Piston aqueous part ECD1 00 0006 B Oo Central CE Piston aprotic part ECD1 00 0005 B Base Flange part ECC1 00 0014 A CE Spring Load _ lM part ECD1 00 0008 A Page 26 of 34 only aqueous REF Electrode II G aaa part ECD1 00 0010 C REF Electrode II E i part ECD1 00 0 C O Ring 21 95x1 78 part DIC9003 ___ O Ring 41x1 78 part DIC9001 valve Support assy part ECD1 00 0004 D _ Countersunk Screw M3x8 part N_7991
10. d 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 Page 19 of 34 EL CELL 6 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 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 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 d On the installation CD run X setup This will install the data logger software Follow any instructions that may appear on your screen e Once installation is finished plug in the provided USB cable into both the host PC and the ECD 2 DL controller box f Launch the data logger software if not already done g After a few seconds the data logger software should report a valid connection and you are ready to st
11. ed CE plunger 2 echnical Specifications 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 e Integrated USB data logger for 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 o Load on working electrode 0 3 N or 1 3 N e Electrolyte volume approx 2 mL Materials in contact with electrolyte PEEK borosilicate glass EPDM rubber stainless steel 316L for aprotic gold for aqueous electrolytes e Operating temperature range Cell and sensor 20 to 70 C Conditioning electronics and data logger 0 to 40 C Page 5 of 34 EL CELL Minimum dimensions for glovebox ante chamber transfer with stand detached Dimensions ECD 2 completely assembled on stand 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 Page 6 of 34 EL CELL 4 Unpacking Check the contents of the packages against the list given below to verify that you
12. f 34 EL CELL Biologic Auxiliary Cable 2 x 2 x 0 14 mm TP shielded Part 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 a to box pt sles D M9 to Biologic AUX Input Pin Signa _ Cable Color Comments 13 Temperature Green 6 _ Anolog IN2 10 10V 200 C V 14 Analog IN1 10 10V ca 50 um V Page 32 of 34 EL CELL 15 Technical Support Technical support for this product is exclusively handled by EL Cell GmbH The following procedure must be followed when the ECD 2 DL or any part of it is returned to EL Cell GmbH for repair 1 2 Page 33 of 34 Send an e mail to info el cell com to obtain a return authorization number and a decontamination report form Sign the decontamination report asserting that the instrument has been decontaminated and is safe for technicians to work on it Describe in detail what is wrong Include a contact name address telephone number and email address Return the instrument to EL Cell GmbH Tempowerkring 6 8 D 21079 Hamburg Germany Email info el cell com EL CELL 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 ma
13. he glass frit 4 Place current collector disc on top of the CE NOTE For aprotic organic electrolytes this disc is not required 5 Insert the central CE piston into the cell bottom O ring size 9 75 x 1 78 mm NOTE For aprotic organic electrolytes use the stainless steel piston instead EL CELL Page 10 of 34 6 Stack cell bottom with central CE piston inserted on top top hold the upside down A flal i Screw the assembly tog Allen screws M4x25 ECD 2_manual 27 02 2015 Put the WE Ol i with the active Page 11 of 34 ECD 2_manual 27 02 2015 12 Place the spac aqueous stainles electrolytes ron top of the WE gold for 316L for aprotic NOTE Three different spacer discs thickness 2 1 2 2 and 2 3 mm are provided to initially adjust the membrane for a given WE thickness close to its neutral flat position see sketch below Use the 2 3 mm disc for a sample thickness between 0 and 150 um WE Spacer disc Metal membrane CE Page 12 of 34 EL CELL 14 Insert the me steel 316L fo 15 Place the cove Page 13 of 34 ECD 2_manual 27 02 2015 16 Fasten the cover screws M4x30 17 Interconnect cell v the numbering on the parts tubing as indicated by 18 Close the side opening NOTE Optionally this auxiliary electrode Page 14 of 34 ECD 2_manual 27 02 2015 EL CELL ye Attach
14. ith 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
15. nalog output cable to the analog input of the respective VMP3 channel In the Biologic EC Lab software load the experiment settings ECD 2 mps provided on the ECD 2 DL 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 EL CELL 9 Dilatometer Disassembly When disassembling the dilatometer cell wear protective gloves and goggles Collect parts that have been in contact with electrolyte on a separate tray for subsequent cleaning In the following order disconnect the cell cable from the dilatometer cell the power supply from the controller box and the sensor cable from the dilatometer cell Remove the dilatometer from the temperature chamber Lock the flexure guide and lift the sensor tip by turning the locking screw 90 clockwise Detach the sensor load unit from the dilatometer cell Detach the cell from the bracket Unscrew the counter electrode spring load Detach the reference electrode Remove the tubing Remove the cover flange the metal membrane the spacer disc and the working electrode Unfasten the cell body and remove the T frit from the cell body 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 othe
16. r solvent After cleaning dry all parts in vacuum at 80 C overnight Additionally dry the cell body and the cell bottom in vacuum at 120 C for at least 12 hours Absorbed moisture may otherwise adversely affect test results Page 22 of 34 EL CELL 10 Using the Reference Electrode The reference electrode assembly is comprised of the reference pin 1 the set collar 2 attached to the pin by means of a set screw 3 the fitting 6 the spring 4 and the hollow screw 5 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 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 6 Fitting 1 7mm with cone 3 Set Screw M2x2 7 Ferrule 1 5 5 Hollow Screw 2 Set Collar 1 7 1 Reference Pin 11 Using an Auxiliary Electrode As an option the ECD 2 DL may be equipped with an additional electrode face to face with the
17. reference electrode This auxiliary electrode may be a second reference electrode or simply a bare metal wire For instance in aqueous solutions a platinum wire auxiliary electrode may be cycled against the counter electrode to determine the actual electrode potential of a simultaneously attached pseudo reference electrode The auxiliary electrode assembly is virtually identical with the reference electrode assembly except that the reference pin is replaced by a metal wire with 1 5 mm diameter 12 Using Single Crystals or Grains as the Working Electrode option With the optionally available Crystal Grain Test Kit part ECD1 00 0018 A the ECD 2 may be loaded with a single crystal or grain as the working electrode Operating Instructions a e Exchange the standard ball tip at the sensor unit with the provided flat tip The tip is connected to the sensor plunger by means of a thread M2 5 For assembly and disassembly the sensor tip must only be turned with your fingertips Never use pliers or other tools as this may damage the sensor unit For cell assembly refer to the instructions given in chapter 5 starting on page 8 In the following only those points are addressed where the assembly differs from the standard procedure Reference is made to the picture step numbers At step 2 account for the height of your sample by placing the provided adjusting washers into the cell body before inserting the T frit The upper thickne
18. ss value in the table below refers to the neutral straight position of the membrane The membrane may be distorted by at least 0 3 mm into vertical direction without causing excessive forces Sample thickness lt 0 1 mm 0 0 1 to 0 4 mm 0 4 to 0 7 mm 0 7 to 1 0 mm At step 11 place one of the provided holed glass fiber separators on top of the glass frit The thickness of the separator must not exceed the sample thickness Then put the sample e g a graphite flake into the separator hole No spacer disc is to be used i e leave out step 12 The holed glass fiber separator may help to improve the wetting of the sample with electrolyte Its use is optional At step 15 place the provided modified cover flange on top The remaining assembly steps and the dilatometer operation are identical with the standard procedure described in chapter 5 Cover flange _ Flat sensor tip Cranked membrane Crystal Sample Adjusting washers Holed GF separator Part Kit for Testing Single Crystals Packing List Flat sensor tip 1 piece T frit borosilicate glass 1 piece Adjusting washer 1 4404 3 pieces Cover flange single crystal 1 4301 1 piece ECC1 01 0021 E X Holed glass fiber separator 10 mm x 0 65 mm 10 pieces ECC1 01 0021 D X Holed glass fiber separator 10 mm x 1 0 mm 10 pieces ECC1 01 0021 C X Holed glass fiber separator 10 mm x 1 55 mm 10 pieces ECC1 00 0019 G Membrane cranke
19. terial 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 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 w
20. the refere for aqueous S pin for a NOTE The ence pi be lo appropria e a e material Dead volume valve red gt Syringe valve yellow 20 Fill the cell withyelectrolyte according to the following procedu Charge a 20 ml syringe with approx 3 ml of electrolyte We recommend one time use PP plastic syringes with low friction polysiloxane pistons Connect the syringe to the Luer adapter of the inner syringe valve 3 Open the syringe valve and close the outer dead volume valve 6 7 Pull the syringe piston back to evacuate the cell Hold the piston a few seconds in the strained position Release the piston so that the electrolyte from the syringe replaces deliberately the previously removed gas NOTE Never pressurize the cell by pushing the syringe piston Repeat the two previous steps to complete filling Close the syringe valve and open the dead volume valve NOTE The cell is now filled and hermetically tight Up to this point for air sensitive systems assembly and filling has to be done in a glove box All subsequent steps may be carried out in ambient atmosphere Page 15 of 34 EL CELL Release the carriage securing the carriage into the uppermost position by turning the micrometer screw clockwise 23 Fasten the sensor lo screws Page 16 of 34 EL CELL Place the dilatometer ins 3 controlled chamber at a stant temperature between 20 to
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