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User Manual - EL-CELL

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1. 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 centre At Sellers 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 mamma SS EL CELL 13 ECC_AIR_manual 11 02 2015
2. Assembly Gas Inlet Siphon Spring PE Washer Seal Locking Ring Gas Outlet Piston REF Sleeve Perforated Current Collector EL CELL 7 ECC_AIR_manual 11 02 2015 6 Operation Modes Gas Supply Thanks to its modular design the ECC AIR test cell 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 simplest set up of this kind the gas 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 connected to the gas outlet For gas analysis the gas outlet may be connected to the continuous gas flow inlet of a mass spectrometer However due to the cell s considerable dead volume and backmixing the time resolution of gas analysis is limited Much better time resolution can be achieved with the ECC DEMS test cell B Dead end pressurized set up In this configuration the gas outlet is plugged and the test cell is pressurized at the beginning of the experiment by means of an external gas supply connected to the gas inlet After equilibration of the closed cell at constant temperature the time constant being mainly determined by the slow dissolution of gases in the electrolyte the cell is charged discharged and the resulting pressure change recorded A gas sample
3. 404 SS 316L and PEEK Other materials available on request e Dedicated tools available to ease cell assembly and operation http el cell com products accessories tools e Modular cell construction with many interchangeable components e Size including bracket 90 mm x 54 mm x 70 mm height x width x depth Weight 640 g 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 Test cell with bracket fully equipped for operation with and without reference 2 PE seals 10 pcs 3 Glass fiber separator 1 55 mm thick 10 pcs ECC_AIR_manual 11 02 2015 4 EL CELL 5 Cell Assembly 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 vert
4. e dried at 80 C in vacuum overnight PE seal and PTFE ferrules are to be replaced NOTE Leaving cell parts in contact with ambient atmosphere while still being wetted with electrolyte may result in Severe corrosion ECC_AIR_manual 11 02 2015 10 EL CELL 9 Accessories and Spare Parts ECC Air Test Cell Ferrule 1 16 Nut part LABOOO2 part ECC1 00 0125 A PEEK Tube part LABOOOS Lid ECC Air Siphon part ECC1i 00 0057 D part ECC1 00 0118 A PE Seal Wina Nut part ECC1 00 0053 A ing Nut assy part ECC1 00 0081 A Locking Washer part ECC1 00 0061 A Compression Spring Au part FED9015 Plunger hole pattern 1 4404 part ECC1 00 0059 C perforated plate part ECC1 00 0114 A Bracket part ECC1 00 0055 A Sleeve Ref WE part ECC1 00 0058 B Separator CE Cell Base part ECC1 00 0056 B Set Collar 1 2 part ECC1 00 0038 B Foot part ECC1 00 0065 A Hollow Screw Socket Screw M4x10 part ECC1 00 0040 A Ferrule 1 0 Spacer part ECC1 00 0029 B part ECC1 00 0064 A Compression Spring Au Fitting 1 1mm with cone part FED9017 Rubber Foot part ECC1 00 0039 D part STD9003 Set Srew Ref Electrode aprotic part N_916_M2x2 part ECC1 00 0062 A mommies EL CELL 11 ECC_AIR_manual 11 02 2015 10 Technical Support Technical support for this product is exclusively handled by EL Cell GmbH The following procedure must be followed when the ECC t
5. electrochemical test equipment Electrochemical Test Cell ECC Air User Manual Release 1 8 2015 02 11 2010 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 Content 1 Product DESCHIOUO Ms cisasccatenceascclacsesbancpdecedsanestaesdnasneductoebiee lt sdcdeduseebisecsaensansanasgenceds 2 2 FOO esee E E E E E E E 3 3 Safety Precautions cc ccccesccssccsssccssecsseccseeceseeesseceeecsseceseeseseeeeeseseseseeeeseeeeees 4 4 RIMS Cr NE eresse e ea eE a a 4 5 Cell Assembly ee 5 6 Operation Modes Gas Supply ccc cccccccscccseccseecsseccsseeeseeesseseseesssesesseesseeeeees 8 7 Electrical Connection 0 0 cece ecccesccssecesceesseceeecsssccseeceseceeecesecesseceseesesseeeeeeseeesees 9 8 Disassembly and Cleaning cccccccsccssccssccsseccseccssecsseesssecsssessseessessseeeseeeegs 10 9 Accessories and Spare Parts cccccsccssccsscessecsseeesseceseesseesssessesessesseeeseeeees 11 10 Technical SUDDO ecoreniroienciareirirar i E E EEEE EREE E EEAS 12 11 Warranty 00 eee ccccsseccssssecesssecessseeeessseeesesecessnseesssseeesssseecesaeeessaeeesesse
6. esssaeeessaaees 13 EL CELL GmbH Tempowerkring 8 D 21079 Hamburg Germany phone 49 0 40 790 12 734 fax 49 0 40 790 12 736 email info el cell com web www el cell com mamma EL CELL 1 ECC_AIR_manual 11 02 2015 1 Product Description The ECC Air is another member of the modular ECC series dedicated to the electrochemical characterization of gas diffusion electrodes in aprotic electrolytes in particular for lithium air batteries Basically the cell accommodates the counter electrode e g Li metal on the cell bottom a gas diffusion electrode on top and a separator in between The upper gas diffusion type electrode is contacted by and breathes through the perforated stainless steel current collector on top The cell lid is equipped with two ports for gas inlet and outlet so that compressed gas can be passed through a siphon along the backside of the gas diffusion electrode The design includes a reference electrode located at the separator s edge Gold plated spring applies reproducible mechanical load on cell stack 10 50 N Stainless steel lid with 2mm banana jacks Inlet Outlet SS 316L piston for corrosion resistance in aprotic media Cutting rings w PE seal ensure ultra low leakage SS 316L base with 2mm Banana Jacks Stainless steel bracket makes assembly fast and easy PEEK sleeve ensures Cell stack Siphon Reference electrode electrode concentricity and assembly ho
7. est cell or any part of it is returned to EL Cell GmbH for repair l Send an e mail to info el cell com to obtain a return authorization number and a decontamination report form 2 Sign the decontamination report asserting that the instrument has been decontaminated and is safe for technicians to work on it 3 Describe in detail what is wrong 4 Include a contact name address telephone number and email address 5 Return the equipment to EL Cell GmbH Tempowerkring 8 D 21079 Hamburg Germany Email info el cell com ECC_AIR_manual 11 02 2015 12 EL CELL 11 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 Sellers 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
8. fusion electrode onto the piston inside the sleeve Put the glass fiber separator into the sleeve and dispense a defined amount of electrolyte onto it The optimum amount of electrolyte 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 Release 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 Connect the inlet port to the gas supply the outlet tube to the exhaust line The provided fittings are compatible with 1 16 inch outer diameter tubing We recommend the use of stainless steel or PEEKsil capillary tubing NOTE Consider using a floating mode potentiostat when grounding the cell lid through metal tubing ECC_AIR_manual 11 02 2015 6 EL CELL Wing Nut Siphon l Lid with 2mm Banana Jacks Gas Inlet Gas Outlet A y a s ie a e r a ra Reference
9. ical position of the reference is determined by the thickness of the components Make sure that the electrodes and separator used have the appropriate thickness to avoid a short circuit between the reference and anyone of the two other electrodes The smaller inside diameter of the reference bore is 0 3 mm Upper Electrode Lower Electrode Assembly Steps I 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 li 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 iii 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 ai EL CELL 5 ECC_AIR_manual 11 02 2015 vi vii viii X xii xiii xiv Put the 18 mm diameter gas dif
10. mogeneous current Perforated distribution plate ECC_AIR_manual 11 02 2015 2 EL CELL 2 Features e Test cell dedicated to the characterization of gas diffusion electrodes in aprotic media e Upper electrode is contacted by and breathes through a perforated current collector e Gas inlet and outlet for supply of pressurized gases to the gas diffusion electrode e A siphon directs the incoming gas to the backside of the gas diffusion electrode e Cell dead volume head space of approx 4 3 cm High precision 18 mm diameter sandwich geometry with lt 0 1 mm electrode concentricity Reliable low leakage sealing with PE seal and PTFE ferrules Temperature operation range 20 to 70 C Easy and reliable electrolyte filling upon assembly Fast assembly and dismantling and easy cleaning of cell components Electrodes are easily accessible for post mortem analysis Reusable cell components except for PE seal Small and defined electrolyte volume due to minimized dead volume Adjustable reproducible and homogeneous mechanical pressure on electrodes 60 FED9021 FED9020 50 FED9015 Std J I T Spring load on stack vs stack thickness for different springs Standard is FED9015 40 4 fg en aed 4 4 4 Spring Load N 00 05 10 15 Stack Thickness mm momma SS EL CELL 3 ECC_AIR_manual 11 02 2015 e Materials in media contact are stainless steel 1 4
11. port valve P N ECC1 00 0155 A is available as an option The sample port may be used to draw gas samples for subsequent analysis or to pressurize the cell at the beginning of the experiment by means of a syringe The ECC PRESS AIR is a version of the ECC AIR featuring a pressure sensor and conditioning electronics to record the pressure evolution inside the cell ECC_AIR_manual 11 02 2015 8 EL CELL 7 Electrical Connection The electrical connection of the test cell to the potentiostat or battery tester is depicted below for 3 electrode operation i e using a reference electrode For 2 electrode operation the RE lead is to be connected to the cell base Note that some potentiostats may not have the CE sense lead WE Sense Ref1 WE CE CE Sense RE WE CA2 CE CA1 Ref3 Ref2 The notations in brackets refer to the standard connection with a Biologic potentiostat MPG 2 SP VSP and VMP series http www bio logic info electrochemistry ec lab instruments Eis CELL 9 ECC_AIR_manual 11 02 2015 8 Disassembly and Cleaning Right after use disassemble the cell in the reverse order of assembly All chemicals used have to be disposed properly Clean wetted parts with water and or other appropriate solvent Ultrasonic cleaning is recommended Persistent dirt on the cell base and plunger may be removed by treatment with aqueous nitric acid 20 2 hours at room temperature After cleaning all parts are to b

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