User Manual - EL-CELL
Contents
1. R meee electrochemical test equipment Electrochemical Test Cell ECC AQU User Manual 2008 2014 Release 2 3 EL CELL GmbH 2014 01 30 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 Contents 1 POO GID SS CDI ene in bi a kapon da ma kek ae ee ia ie 3 Ze OU eS vs gress alye v ti atea E ei n la ali a is e ke cain e ones 4 3 SAMEM FI ECIUTNON S ses ass EEEk 5 CAC RICE kitte te bade det ja e li ee a e m ka in e n a e e are pe 5 5 ECC ASS SN aa d at ae ue mn ee 7 5 1 AAA OG RE yd tiye tit eny RER TES 7 5 2 AAA Reference Mode 9 5 3 ABA NO aa a sn cn 0 11 5 4 ABA Vacuum Mode 12 6 Accessories and Spare Parts 14 Ta AMOR see akt n konn l kap a s ee any 16 8 Technical Support ll llleelteeltteetteettaettaeeteaeoseoooseooseoooooooseooooooooooonons 16 I MWAN AN MY krie at onn n a ae lese en anle y E De p e ize ae loi as 17 EL CELL GmbH Tempowerkring 8 D 21079 Hamburg Germany phone 49 0 40 790 12 733 fax 49 0 40 790 12 736 info el cell com www el cell com Page 2 of 17 EL CELL 1 Product Description The ECC cell design is the result of man2. AQU test cell in the AAA mode with reference pin assembly Detail view of the reference pin assembly Page 10 of 17 ECC_AQU_manual 30 01 2014 EL CELL 5 3 ABA Mode In the ABA mode the cell is assembled with a thin separator that is larger in diameter than the two adjacent electrodes so as to prevent a short circuit along the edge of the thin separator An alignment tool is provided to ensure concentricity of the two sandwich electrodes upon assembly Upper Electrode Lower Electrode Assembly Steps Close the side opening of the cell base with the provided plug Insert the piston into the sleeve and hold the piston sleeve assembly with the contact face of the piston pointing upwards Place the gold current collector disc and the working electrode on top of the piston inside the sleeve Dispense a defined amount of electrolyte onto the electrode About 0 3 mL of electrolyte is appropriate for 0 1 mm thick components electrodes and separator Place the 20 mm separator on top of the wetted electrode Make sure that the electrode is fully covered by the separator Attach the provided alignment tool and insert the counter electrode and finally the second gold current collector on top of the stack Detach the alignment tool Push the cell base over the assembly press onto the piston and turn the cell into the upright position Mount the spring and the PE seal Attach the cell lid insert the cell into the bracket and tighte
3. EL gt part ECC1 00 0053 A Compression Spring Au gt part FED9015 9 2mm _ LI k Thrust Screw ort part ECC1 00 0066 A ep Wing Nut assy part ECC1 00 0081 A ee Bracket part ECC1 00 0055 A Cell Base aqueous part ECC1 00 0068 A Set Collar 1 2 part ECC1 00 0038 B Hollow Screw part ECC1 00 0040 A Compression Spring Au part FED9017 Set Screw M2x2 part N 913 Ref Electrode 1 0mm aqueous part ECC1 00 0062 E Feed Wire part ECC1 00 0071 A Page 15 of 17 Foot part ECC1 00 0065 A Spacer part ECC1 00 0064 A Socket Screw M4x10 part N_912 Rubber Foot part STD9003 Ferrule part LAB0007 Set Screw M2x2 part N 913 Touch Screw part ECC1 00 0072 A EL CELL 7 Maintenance Right after disassembly all materials used have to be disposed properly All wetted parts are to be cleaned with an appropriate detergent wash and solvent water ethanol or acetone The transfer line used for filling the cells is to be purged with the aid of a syringe All parts are to be dried immediately after cleaning in vacuum at 80 C PE seals and O rings are to be replaced NOTE Leaving cell parts in contact with ambient atmosphere while still being wetted with electrolyte may result in severe corrosion 8 Technical Support Technical support for this product is exclusively handled by EL CELL GmbH The following procedure must be followed when the ECC test
4. cell or any part of it is returned to EL CELL GmbH for repair 1 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 Web www el cell com Page 16 of 17 EL CELL 9 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 resulti
5. G9005 allen wrench 0 9 mm 14 EGC1 00 0069 A Current collector Au 15 ECC1 00 0092 A Sleeve removing tool 16 EGC1 00 0053 A PE seal 10 pcs 17 EGC1 01 0012 C Glass fiber separator 18 x 1 55 mm 10 pcs 18 EGC1 00 0022 B Separator Celgard 2325 20 x 0 025 mm 10 pcs picture see next page Page 5 of 17 EL CELL Page 6 of 17 ECC_AQU_manual 30 01 2014 5 ECC Assembly The ECC electrochemical cell may be operated in several modes which differ in the size of the components used diameter and thickness and in the way the cell is filled with electrolyte dropping onto separator during assembly or vacuum filling afterwards NOTE In order to remove oxygen the fully assembled cell with the side opening unplugged may be out gassed in a vacuum oven prior to filling it with de aerated electrolyte via the syringe method Assembly and filling ina glove box is possible as well 5 1 AAA Mode In this mode the cell is assembled with a thick fiber cloth separator having the same 18 mm diameter as the two adjacent electrodes and a thickness of between 0 2 and 2 mm The cell is filled with the electrolyte during assembly by dropping a given volume of electrolyte directly onto the separator 0 1 to 1 ml depending on the separator and electrodes used Only when applying the spring load upon final cell closure a defined amount of electrolyte is squeezed out of the separator and soaks the two adjacent electrodes The confine
6. e assembly mode Page 3 of 17 EL CELL 2 Features Page 4 of 17 High precision 18 mm diameter sandwich geometry with lt 0 1 mm electrode concentricity Reliable ultra low leakage with PE seal Temperature operation range 40 to 80 C wider ranges on request Easy and reliable electrolyte filling either upon assembly or afterwards via syringe vacuum method Fast assembly and dismantling and easy cleaning of cell components Electrodes are easily accessible for post mortem analysis Reusable cell components except for PE sealing Small and defined electrolyte volume down to 0 05 cm Equipped with reference pin assembly for three electrode operation Adjustable reproducible and homogeneous mechanical pressure on electrodes 60 FED9021 FED9020 50 FED9015 Std Spring load on stack vs stack thickness for different springs Standard is FED9015 p w t OUE ma me mm _ Lo mi an Spring Load N O 0 0 0 0 5 1 0 Stack Thickness mm 1 5 Materials in media contact are gold and PEEK other materials on request Modular cell construction with many interchangeable components Plug and play multi cell fixture available for operation inside temperature chamber or wall mounting and for connection to a multi channel potentiostat or battery tester Size including bracket 90
7. eston Std sleeve Piston W Cell base Plug assembly out SR es er pa a pe cu wn ton ane Seg a lan Cell stack ECC AQU test cell in the AAA assembly mode Page 8 of 17 EL CELL 5 2 AAA Reference Mode In the reference mode a metal pin is to be positioned close to the separator edge in between the working and the counter electrode This metal pin can either function directly as the reference electrode e g when using a silver wire coated with silver chloride or the inert metal pin makes the electronic contact with some reference material that is to be loaded upfront into the feed through hole of the REF sleeve The ECC AQU test cell is equipped for the second case and the corresponding cell assembly is described below The reference material has to be provided by the user We have good experience with using PTFE bound activated carbon as the reference material when working with neutral and acidic electrolytes not suited for alkaline electrolytes Depending on the type of reference material used it may be advised to enlarge the small feed through hole of the REF sleeve 0 3 mm diameter standard with the aid of a hand drill or to pre load the small feed through hole of the REF sleeve with a piece of fiber cloth Serving as an electrolyte wick Please consult us for more specific information Note that the use of conventional reference electrodes is restricted by the narrow diameter of the feed through
8. ge with ca 0 3 ml of electrolyte b Connect the syringe via the transfer line to the side opening of the cell c Push the syringe piston back to evacuate the cell Hold the piston a few seconds in the strained position d Hold the syringe with the piston upwards and release the piston so that the electrolyte is drawn into the cell e Repeat the two previous steps to complete filling if necessary f Remove the syringe together with the transfer line and close the cell with the provided plug Page 12 of 17 EL CELL Wing nut Syringe Bracket Lid PE seal Std sleeve Piston Internal O Ring seals Cell base Transfer line SS ECC test cell in the ABA vacuum mode 6 Accessories and Spare Parts ECC AQU with syringe for vacuum filling transfer line f ECC series Set part ECC1 01 0001 A gt PTFE Plug assy 1 10 part ECC1 00 0130 A Page 14 of 17 EL CELL Locking Washer part ECC1 00 0061 A Set Screw M2x2 part N_913 Feed Wire part ECC1 00 0071 A Ferrule part LABOOO7 Central Upper Piston aqueous part ECC1 00 0080 A Sleeve Ref part ECC1 00 0058 B Current Collector 18mm part ECC1 00 0069 A WE Separator CE Current Collector 18mm part ECC1 00 0069 A ECC AQU with reference pin assembly gt PE Seal Insulation Ring Seal Insulation Ring a n part ECC1 00 0053 A r Lid part ECC1 00 0057 A SS a PE Seal
9. hole in the cell base which ts only 1 6 mm Upper Electrode Lower Electrode Assembly Steps Load the feed through hole of the REF sleeve with a small piece ofthe fiber cloth if applicable and subsequently the reference material dedicated tool the ECC RefLoad is optionally available to ease this assembly step http el cell com products accessories tools ecc load ii Insert the piston into the sleeve and hold the piston sleeve assembly with the contact face of the piston pointing upwards lil Place the gold current collector disc the working electrode and the fiber cloth separator on top of the piston inside the sleeve Chose the thickness of the separator so as to avoid a short circuit between the reference and one of the two sandwich electrodes iv Dispense a defined amount of electrolyte onto the separator v Place the counter electrode and finally the second gold current collector on top of the stack inside the sleeve Vi Push the cell base over the assembly press onto the piston and turn the cell into the upright position vii Mount the locking ring the spring and the PE seal vill Screw the reference assembly into the side opening of the cell base IX Attach the cell lid insert the cell into the bracket and tighten the wing nut Page 9 of 17 EL CELL Wing nut Bracket Lid Spring REF sleeve Locking washer Cell base Piston Reference pin assembly Cell stack ECC
10. ment of the cell stack by an insulating sleeve ensures a homogeneous current distribution and thus makes this configuration ideal for impedance measurements Upper Electrode Lower Electrode Assembly Steps I Close the side opening of the cell base with the provided plug ii Insert the piston into the STD sleeve and hold the piston sleeve assembly with the contact face of the piston pointing upwards iii Place the gold current collector disc the working electrode and the fiber cloth separator on top of the piston inside the sleeve iv Dispense a defined amount of electrolyte onto the separator v Place the counter electrode and finally the second gold current collector on top of the stack inside the sleeve vi Push the cell base over the assembly press onto the piston and turn the cell into the upright position Page 7 of 17 EL CELU vii Insert the spring and the PE seal vili Attach the cell lid insert the cell into the bracket and tighten the wing nut Note The appropriate amount of electrolyte depends on the porosity and thickness of the components used and thus has to be determined in pre tests The amount must be smaller than the absorption capacity of the separator in its uncompressed state 0 5 mL of electrolyte is a good starting value when using the 1 5 mm thick standard separator and electrodes of around 0 1 mm thickness Ae Wing nut Bracket Lid Spring PE seal n FT et re w w
11. mm x 54 mm x 70 mm height x width x depth Weight ca 600 g Dedicated tools available to ease cell assembly and operation http el cell com products accessories tools 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 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 Purchased parts package ECC Aqu ECC1 00 0006 A ECC1 00 0200 A Cell bracket wing nut assembly ECC1 00 0068 A Cell base aqueous ECC1 00 0057 A Cell lid ECC1 00 0130 B PTFE plug ECC1 00 0058 A Sleeve Std ECC1 00 0080 A Central upper piston aqueous ECC1 00 0053 A PE Seal FED9015 Compression spring gold plated Co ae a Accessories kit ECC1 00 0303 A 9 ECC1 00 0010 C Reference pin Au for 3 electrode operation replaces PTFE plug assembly 10 ECC1 00 0058 B Sleeve Ref for 3 electrode operation replaces Std sleeve 11 ECC1 00 0091 A Adjustment tool for ECC Aqu for electrode alignment in the ABA assembly mode 12 ECC1 00 0061 A Locking washer 13 WZ
12. n the wing nut Page 11 of 17 EL CELL 5 4 ABA Vacuum Mode The ABA vacuum mode is recommended when working with experimental electrolytes that do not easily wet the electrodes or separator used O ring seals are to be mounted to both piston and STD sleeve in order to apply vacuum during the final electrolyte filling procedure Note that the O ring seals and the syringe transfer line required for vacuum filling have to be ordered separately Assembly Steps vii viii iX Mount O ring seals to piston and STD sleeve Leave the side opening of the cell base unplugged Insert the piston into the sleeve and hold the piston sleeve assembly with the contact face of the piston pointing upwards Place the gold current collector disc and the working electrode on top of the piston inside the sleeve Place the 20 mm separator into the recess of the sleeve on top of the dry electrode Make sure that the electrode is fully covered by the separator Attach the provided alignment tool and insert the counter electrode and finally the second gold current collector on top of the stack Detach the alignment tool Push the cell base over the assembly press onto the piston and turn the cell into the upright position Mount the spring and the PE seal Attach the cell lid insert the cell into the bracket and tighten the wing nut Fill the cell by means of the syringe vacuum method according to the following procedure a Charge a5 ml syrin
13. ng 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 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 Page 17 of 17 EL CELL
14. y years of experience and iterative improvement in battery and supercapacitor electrode testing It is perfectly suited for voltammetry and impedance as well as cycle life testing The ECC Aqu Electrochemical Cell is another member of the modular ECC test cell series dedicated to the characterization of aqueous battery systems All metal parts of the ECC Aqu test cell that come into contact with the electrolyte are made of gold Other metals like platinum or tantalum are optionally available and may be easily replaced by the user The ECC Aqu cell is equipped with a reference pin assembly to control or monitor half cell potentials This manual covers the aqueous test cell ECC Aqu A separate manual is available for the two aprotic test cell versions ECC Std and ECC Ref Stainless steel bracket for easy assembly fits into multi cell Gold plated spring m EE docking station ECC Stand applies reproducible lm mechanical load on cell stack 10 50 N Stainless steel lid with 2 mm banana jacks 4 fold cutting rings with PE seal ensure ultra low PEEK piston with gold gt 4 Mh leakage wire lead through towards upper gold current collector PEEK sleeve ensures electrode concentricity and homogeneous current distribution Reference pin assembly PEEK base Gold wire lead through towards Cell stack lower gold current collector with 2 mm banana jack ECC Aqau test cell in the AAA referenc
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