User Manual - EL-CELL
Contents
1. Analog Out Cable T Chamber Page 12 of 23 EL CELL 8 Sample Valve with Septum Port The gas sample valve serves to draw gas samples from the head space of the ECC Press Air test cell In the closed state the valve spindle is seated on the PTFE ferrule and is thus preventing any bleeding from inside the cell through the septum In order to draw a gas sample pierce the septum with the sample syringe ii open the valve by turning the valve handle counter clockwise by 90 degrees iii charge the syringe IV close the valve by turning the valve handle clockwise till finger tight and remove the syringe Valve Handle PTFE Ferrule Valve Seating Valve Stem Septum Septum Port Page 13 of 23 EL CELL 9 Software Installation DL option The ECC Press Air DL features an integrated USB data logger for recording cell pressure temperature cell potentials and current The software installation on a Windows PC is described below 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 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 the2. 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 equipment to EL CELL GmbH Tempowerkring 8 D 21079 Hamburg Germany Email info el cell com Page 22 of 23 EL CELL 15 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 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 o
3. C Air Gas Sample Port assy part ECC1 00 0057 D part ECC1 00 0155 A PE Seal part ECC1 00 0053 A Locking Washer part ECC1 00 0061 A Siphon part ECC1 00 0118 A Transfer line assy part ECC1 01 0001 C Jackshaft er part ECC1 00 0081 A Bracket part ECC1 00 0055 A Compression Spring Au part Sr Ur Loam Plunger hole pattern 1 4404 part ECC1 00 0059 C Sleeve Ref part ECC1 00 0058 B Perforated Plate part ECC1 00 0114 A WE Separator CE Cell Base part ECC1 00 0056 B 8 Qf Ref Electrode ECC assy Page 18 of 23 EL CELL Gas sample port assy ECC1 00 0155 A O Ring 2x1 Septum part DIC9021 part ECC1 00 0097 A Valve Seating part ECC1 00 0153 A Ferrule 1 0 part ECC1 00 0029 B Valve Stem Septum Thrust Screw II part ECC1 00 0063 A part ECC1 00 0098 B Page 19 of 23 EL CELL Reference pin assy ECC1 00 0010 D Set Collar 1 2 Set Srew M2x2 Hollow Screw part ECC1 00 0038 B part N 916 M2x2 part ECC1 00 0040 A amp y Compression Spring Au part FED9017 Ref Electrode Ni aprotic part ECC1 00 0062 A Fitting 1 1mm with cone part ECC1 00 0039 D Ferrule 1 0 part ECC1 00 0029 B Page 20 of 23 EL CELL 13 Cables and Connectors Cable Color 1 Vi Red mRedplug Blue plug 3 Grey plug Yellow plug Ld E o o o ee E a a sensor plug housing Brown gj Sduare sensor plug De d S Plug Color ed T VTEMP2 Red __ 0 10
4. EL CELL electrochemical test equipment Electrochemical Test Cell ECC Press Air DL User Manual Release 1 4 2012 2015 2015 02 11 EL CELL GmbH PCB ECC PRESS DL 1 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 Content 1 Product DESCLIDTION c ccc ceecceecseeeeeeceeeeeeeeeeseeeseeeeeesaeeseeeeeeseeens 3 2 Features and Specification cccccccccecccceececeececeeeeseeeesseeesaeeeeees 3 3 Safety Precautions cccccccccsscecseeeeseecseeeeeeteeeeaeeeteueeeeeteneeseeetes 7 Ar NIWA AC IMG mE u 7 5 Cell Assembly ee 8 6 Operation Modes Gas Supply eeeeeeeeeeeeeeese 11 7 Electrical Connection eeeeseeseeeseeeneeeeenneenen rn 11 8 Sample Valve with Septum PoOMt cccccseeeeeeeeceeeeeeeeeseeeeeaeeees 13 9 Software Installation DL option eeeeseeeeees 14 10 Recording the Pressure Signal with an External Potentiostat 14 11 Disassembly and Cleaning eeeeeeeeeeeeeeeee 16 12 Accessories and Spare Parts cccc
5. SA15R 240P mains adapter Analog output voltages 0 to 10V 1 kOhm 100 nF for pressure and temperature Resolution of pressure analog output 0 0596 of measurement range Error of pressure analog output 0 596 of measurement range comprising non linearity including hysteresis and non reproducibility Resolution of temperature analog output 0 01 C Error of temperature output 1 C Optional USB data logger powered by host PC with galvanic isolation Operating temperature range controller 0 to 40 C Page 6 of 23 EL CELL 3 Safety Precautions Use proper safety precautions when using hazardous electrode materials and electrolytes Wear protective glasses and gloves to protect you against electrolyte that may accidentally spill out during filling and disassembly Upon cell disassembly dispose all materials properly Metallic lithium and some insertion compounds may decompose heavily in contact with water and other solvents and can cause fire 4 Unpacking Check the contents of the packages against the list given below to verify that you 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 1 ECC Press Air test cell with pressure sensor assembled for use in a 2 electrode dead end pressurized set up 2 Gas sample port with septum and valve 3 Reference
6. V 40 C V ES ooo opo amp ooo oo P VP2 0 10V 0 25 bar V ee G S y 9 GND Black Common ground Page 21 of 23 Cell Cable 6x2 twisted pairs Sub D M15 HD connector to box 2 mm banana plugs and square sensor plug M16 to ECC PRESS test cell shield connected to Sub D connector housing and to sensor housing Pt100 sensor located inside sensor plug housing Part No ECE1 00 0032 B Analog Out Cable Sub D F9 connector to box 2 mm banana plugs for connection to external devices Part No ECE1 00 0040 A EL CELL Biologic VMP3 Auxiliary Cable 2 x 2 x 0 14 mm TP shielded Sub D F9 connector to box Sub D M9 connector to auxiliary input connector of the Biologic potentiostat The cable shield is tied to both connector housings Part No ECE1 00 0040 B Sub D HD F15 to box oo Sub D M9 to Biologic AUX Input Cable Color Comments 2 T VTEMP2 Red 6 Analogln2 _0 10V 40 C V 4 1 dl d EO 8 o o o o O7 es G C a oO e o S ooo oo 9 GND Bown 7 GND O 14 Technical Support Technical support for this product is exclusively handled by EL CELL GmbH The following procedure must be followed when the ECC test cell or any part of it is returned to EL CELL GmbH for repair ls 2 eS Send an e mail to info el cell com to obtain a return authorization number and a decontamination report form Sign the decontamination report
7. ccccceecccsceseeeeeeeeeeeeeeseeeeens 17 13 Cables and Connectors eesseesseeeseeenneeneenennnn 18 14 Technical Support cccceccceccceeecceeeseeeeceeeeeeeeseeeeseeseueeseeesanees 22 IN eu m 23 EL CELL GmbH Tempowerkring 8 D 21079 Hamburg Germany phone 49 0 40 790 12 734 fax 49 0 40 790 12 736 info el cell com www el cell com Page 2 of 23 EL CELL 1 Product Description The ECC Press Air test cell is dedicated to the characterization of gas diffusion electrodes in aprotic electrolytes in particular for lithium air batteries The attached pressure sensor serves to monitor the inside pressure in either a flow through or in a dead end pressurized set up The ECC Press Air combines all the features of the ECC Press and the ECC Air test cells The provided low dead volume sampling port valve serves to draw gas samples from the cell s headspace The cell hardware is based on the ECC Std and ECC Ref test cells and can be used with or without a reference electrode The ECC Press Air comes with a controller box for easy interfacing with an external potentiostat The box provides analog outputs for both pressure and temperature As an option all relevant signals of the experiment cell pressure temperature cell potentials and current may be recorded with an integrated USB data logger DL option Pressure sensor 0 to 2 5 bar abs Variable dead volume by mea
8. e the ECC Press Air inside a temperature controlled chamber at a constant temperature between 20 to 70 C The chamber needs to have a feed through for cable connection to the controller box outside the chamber Inside the chamber attach the square sensor plug to the pressure sensor and connect the 2 mm banana plugs of the cell cable to the cell red and green to the lid blue and yellow to the base black to the reference Page 11 of 23 EL CELL Outside the chamber connect your potentiostat to the 4 mm banana sockets 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 Biologic Potentiostat Box Potentiostat ME etc WE Current Both the pressure and the temperature signals are available at the Analog Out connector of the controller box These signals can either be routed to the analog inputs of the controlling potentiostat if available or to some other recording device The pressure is linearly related to the pressure sensor voltage according to P abs 0 25 bar V Voltage Likewise the temperature is related to the temperature sensor voltage according to T 40 CO V Voltage ECC PRESS DL USB Cable Cell Cable amp e t T KA nas i Cr 6e L Controller Power Supply
9. electrode pin REF sleeve and locking pin for 3 electrode operation 4 PE seals 10 pieces 5 Septum 10 pieces 6 One way syringe and needle 7 Glass fiber separators 18 mm x 1 55 mm 10 pieces 8 Sleeve removal tool 9 24 V power supply with country specific adapters 10 Controller box with analog outputs for pressure and temperature 4 mm banana sockets for connection to an external potentiostat and integrated USB data logger DL option 11 CD with manual and data logger software DL option 12 USB cable DL option 13 Cell cable for connection between test cell and controller box Page 7 of 23 EL CELL 5 Cell Assembly The test cell can either be operated in 2 electrode or 3 electrode reference configuration In the following the cell assembly is described for operation with a lithium metal reference electrode Generally all assembly steps are to be carried out in inert glove box atmosphere and all components used are to be dried upfront in a vacuum oven at 80 C for at least 12 hours The pressure sensor together with the transfer line may remain permanently attached to the stand In order to operate the test cell with a reference the small feed through hole of the REF sleeve is to be loaded with the reference material usually metallic lithium The vertical position of the reference is determined by the thickness of the components Make sure that the electrodes and separator used have the Upper Electrode appro
10. implest set up of this kind the cell inlet is connected to the gas oxygen supply via a mass flow controller and the pressure build up inside the cell is controlled by means of a metering valve or narrow capillary at the gas outlet located at the sensor adapter For gas analysis the gas outlet may be connected to the continuous gas flow inlet of a mass spectrometer A small dead volume and plug flow conditions are mandatory for a good time resolution of the gas analysis This is achieved by having all spacers installed inside the test cell and in the sensor adapter Even better time resolution is possible with the ECC DEMS test cell B Dead end pressurized set up In this configuration the gas outlet at the sensor adapter is plugged and the test cell is pressurized at the beginning of the experiment through the attached sample valve port After equilibration of the closed cell at constant temperature the time constant mainly determined by the slow dissolution of gases in the electrolyte the cell is charged discharged and the resulting pressure change is recorded For a given amount of gas the magnitude of pressure change is the larger the smaller the dead volume The gas composition may be analysed by drawing gas samples via the attached sample valve port However for gas analysis the dead volume spacer in the sensor adapter must be in place in order to avoid concentration gradients Electrical Connection For best results plac
11. is recommended Persistent dirt on the cell base and plunger may be removed by treatment with aqueous nitric acid 2096 2 hours at room temperature All parts are to be dried immediately after cleaning at 80 C It is recommended to leave the pressure sensor together with the transfer line attached to the stand Typically these parts need not be disassembled or cleaned NOTE Leaving cell parts in contact with ambient atmosphere while still being wetted with electrolyte may result in severe corrosion Page 16 of 23 EL CELL 12 Accessories and Spare Parts ECC Press Air DL complete Test Cell assy Sample Port assy part ECC1 00 0155 A PTFE Plug assy Cap Nut M4 C LEER part ECC1 00 0130 B part N 1587 N ut og AS N f Cy Reference Electrode PTFE MXN EZ art ECC1 00 0010 E Pressure Transducer SA di i part SEN9020 U Scheibe 4 1 10 1 PE Seal part SON9010 part ECC1 00 0095 A Dead volume spacer B part ECC1 00 0136 A Insulating Bush po ee part SON9007 Dead volume spacer A Q v 9 part ECC1 00 0135 A A AS Socket large volume A part ECC1 00 0094 B Socket screw part N_912 Interlock part ECC1 00 0096 B Stand part ECC1 00 0096 A Hex Nut m18 part N_439 Rubber Foot part STD9003 Insulating Bush M4 part SON9008 Countersunk Socket Screw M4x8 Rubber Foot part N_7991 part STD9003 Page 17 of 23 EL CELL Test Cell assembled as 3 electrode cell Lid EC
12. m Visualised dead volume both spacers installed delivery condition 3 024 cm Page 4 of 23 EL CELL e Optional integrated USB data logger for recording of cell pressure temperature cell potentials and current DL option e Operation in either flow through or dead end pressurized set up e Fully equipped for operation with and without reference electrode e Reliable ultra low leakage sealing with PE seal e High precision 18 mm diameter sandwich geometry with 0 1 mm electrode concentricity e Operating temperature range 20 to 70 C cell e Easy and reliable electrolyte filling upon assembly e Fast assembly and dismantling and easy cleaning of cell components e Electrodes are easily accessible for post mortem analysis e Reusable cell components except for PE seals e Small and defined electrolyte volume down to 0 05 cm e Adjustable reproducible and homogeneous mechanical pressure on electrodes e Materials in media contact are stainless steel 1 4404 and PEEK other materials on request e Modular cell construction with many interchangeable components e Size including stand 90 mm x 80 mm x 240 mm height x width x depth e Weight 900g e Dedicated tools available to ease cell assembly and operation http el cell com products accessories tools Dimensions Cell 280 A L HHS An m I LZ 9 Page 5 of 23 EL CELL Electrical Specifications Controller Input 24V 0 6A supplied by P
13. ns of two sensor spacers Port plugged or for gas outlet Sampling valve with syringe port or port for gas inlet Stand wall mountable ECC Air test cell i Reference pin Page 3 of 23 EL CELL 2 Features and Specification ECC Press Air test cell dedicated to the characterization of gas diffusion electrodes in aprotic media Upper electrode is contacted by and breathes through a perforated current collector Gas inlet and outlet for supply of pressurized gases to the gas diffusion electrode A siphon directs the incoming gas to the backside of the gas diffusion electrode Sampling valve with septum port for drawing gas samples by means of a syringe Attached pressure sensor for monitoring of inside gas pressure Default pressure range of O to 2 5 bar absolute Conditioning electronics with analog outputs for pressure and temperature for seamless integration with external instrumentation Total dead volume variable between 4 448 cm both sensor spacers in place and 16 917 cm without spacer Deadvolumein cm 1 Both spacers installed 4 448 2 Only ECC1 00 0136 A sensor spacer B installed 10 582 3 Only ECC1 00 0135 A sensor spacer A installed 10 783 4 No spacer installed 16 917 delivery condition Requires de mounting of the sensor and must be done at factory Dead volume spacer B Dead volume spacer A part ECC1 00 0136 A part ECC1 00 0135 A Volume 6 134 cm Volume 6 335 c
14. priate thickness to avoid a short circuit between the reference and anyone of the Separator two other electrodes The smaller inside diameter of the reference bore is 0 3 mm Lower Electrode Assembly Steps 1 Make sure that the siphon is properly attached to the cell lid For this purpose plug the siphon into the cell lid with the siphon side bore pointing to the gas Outlet port in the lid Then attach the tube transfer line to the gas outlet port so that the tube end fits into the side bore and thus holds the siphon in place ii Pick up a small piece of lithium by a metal wire and press the lithium into the feed through hole of the REF sleeve until the lithium Just arrives at the inner face of the sleeve Note that significant force has to be applied to achieve that A special REF loading tool is available for this purpose not included lil Close the side opening of the cell base with the provided plug This plug is later on replaced by the reference pin IV Assemble the two part WE piston with the perforated current collector pointing upwards V Insert the WE piston into the sleeve with the perforated current collector pointing upwards vi Put the 18 mm diameter gas diffusion electrode onto the piston inside the sleeve Page 8 of 23 EL CELL vii viii xi xii xiii Put the glass fibre separator into the sleeve and dispense a defined amount of electrolyte onto it The optimum amount of electrol
15. provided USB cable into both the host PC and the ECC PRESS AIR 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 start the measurement The calibration data and 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 Additional information on the EC LINK software can be found in the EC LINK Quick Start Guide 10 Recording the Pressure Signal with an External Potentiostat Many of today s battery testers and potentiostats provide additional analog inputs that may be used to record sensor signal along with cell current and potential In the following the combination of the ECC Press Air 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 pressure and temperature Page 14 of 23 EL CELL 1 Connect the 9 pin Sub D connector of the optional analog output cable to the analog input of the respective Biologic VMP3 channel 2 In the Biologic EC Lab software in the Cell Characteristics dialog click on Record external de
16. r service centre 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 oeller 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 Page 23 of 23 EL CELL
17. vices Hecord E Ecen WE CA2 Pw ret 1 Analog IM 17 fe payee Analog IN 2 Record external devices on Analog H3 refs Fies LE DAT 3 Inthe External Devices Configuration dialog chose Device Type Other and define a Custom Variable Pressure bar Then fill in the conversion parameters in the MEASURE fields as shown below External Devices RDE Configuration Device Type Device Mame Other Other Analog OUT Analog IM 1 L Convert TAC to EA Convert E V Pressure bar with Hon E wma with Ao Vv 25 bar max oF rnin 0 w D bar iy Manual Control Analog IN 2 TPC foo 4 Convert EA TAC with 25 V 100 C max 0 wv O Cimin 0 Custom Variables OF Cancel 4 Click OK to close the External Devices Configuration Record Brel WE CAZ PP ref v Pressure bar on Analog IM 1 RE ret we 4 TAC on amp nalog IN 2 Record external devices on Analog INF refs CECA Files For convenience the ECC Press Air documentation CD contains the above settings in the EC Lab setting file ECC PRESS mps Page 15 of 23 EL CELL 11 Disassembly and Cleaning Right after use disassemble the cell in the reverse order of assembly Note that the reference pin MUST be detached before the REF sleeve can be removed All chemicals used have to be disposed properly All wetted parts are to be cleaned with water and or other appropriate solvents Ultrasonic cleaning
18. yte depends on the electrodes and separator used and has to be carefully determined in pre tests 0 5 cm are a reasonable amount for 1 5 mm thick glass fiber separator Put the lithium CE disc 18 mm diameter approx 0 2 mm thick on top of the cell stack Push the cell base over the assembly hold the components tightly together and turn the assembly back into the upright position Helease the pressure applied on the cell stack mount the locking ring to align the side opening of the cell base with the feed through hole of the REF sleeve and replace the plug in the cell base by the spring loaded REF pin Insert the PE seal and the spring Attach the cell lid with the siphon and tube already attached Push the cell into the bracket and tighten the wing nut Page 9 of 23 EL CELL erem rmi mr Wing Nut Lid with 2mm banana jacks Gas inlet or gas sample port valve Connection line to pressure sensor eos le Stren eT EUM patie Siphon e Spring PE seal Locking ring Cell base with 2mm Piston banana jacks REF sleeve Reference assembly Perforated current collector Cell stack Page 10 of 23 EL CELL 6 Operation Modes Gas Supply Thanks to its modular design the ECC Press Air may be operated in different modes Two basic set ups are described below A Flow through set up This is the most typical configuration for the characterization of Li air batteries In the s
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