User Manual - EL-CELL
Contents
1. Cover the graphite sample material with one of the provided 16 mm current collectors meshes Insert the upper O Ring seal 16 x 1 8 mm into the cell body and place the optical window on top Make sure that the window is in the center position Attach the lid and fasten the three socket screws Attach the WE contact pin to port A Attach the reference pin to the reference port Plug the reference port if working without reference electrode Attach the touch screw from below and raise it to the uppermost position then turn the touch screw back counter clockwise by about 30 Fill the cell with electrolyte according to the following procedure Connect the provided filling tube to port B Charge a 5 ml syringe with ca 0 5 ml of electrolyte NOTE We recommend one time use PP plastic syringes with low friction silicone pistons EL CELL User Manual ECC Opto Std Release 2 3 Page 9 of 19 Connect the syringe to the Luer adapter of the filling tube Pull the syringe piston back to evacuate the cell Hold the piston a few seconds in the strained position The syringe piston must be kept with the opening facing downwards The gas is drawn through the electrolyte out of the cell This can be identified by the bubbles in the electrolyte Release the piston so that the electrolyte is being drawn deliberately into the cell NOTE Never pressurize the cell during the filling procedure Repeat the two previous2. 1 Zinc Selenide window 22 x 0 3 mm ECC1 00 0250 B s 2 Lid Zinc Selenide ECC1 00 0127 E Components Calciumfluoride Kit ECC1 00 0156 E 1 Calciumfluorid window 22 x 0 3 mm ECC1 00 0250 C 2 Lid Calciumfluorid ECC1 00 0127 E EL CELL User Manual ECC Opto Std Release 2 3 Page 15 of 19 9 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 10 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 abus
3. of 19 7 X Ray Experiments For X ray experiments the optional XRD Kit is available ECC1 00 0156 B The XRD kit comprises a Beryllium window ECC1 00 0222 A and a modified cell lid ECC1 00 0127 C The lid features a 10 mm wide groove that allows for a viewing angle onto the sample surface as low as 8 Lid with groove List of Components X ray Kit ECC1 00 0156 B 1 Beryllium window 22 x 0 2 mm ECCi 00 0222 A 2 Lid XRD ECC1 00 0127 C EL CELL User Manual ECC Opto Std Release 2 3 Page 13 of 19 Viewing angle X Ray Kit Lid with groove Current collector mesh foil with Beryllium window working electrode on top At very positive potentials the Beryllium window may suffer from oxidation In this case we recommend placing a thin insulation layer e g a small piece of polyethylene foil 15 mm in diameter 10 um thick in between the holed current collector and the Beryllium window Beryllium is highly toxic and can cause cancer Take proper precautions when handling the Beryllium window Avoid direct contact with skin Carefully collect and dispose properly any Beryllium fragments when accidentally breaking the window EL CELL User Manual ECC Opto Std Release 2 3 Page 14 of 19 8 Further Kits Components Sapphire Kit ECC1 00 0156 C 1 Sapphire window 22 x 0 3 mm ECC1 00 0149 A 2 Lid Sapphire ECC1 00 0127 B Components Zinc Selenide Kit ECC1 00 0156 D
4. 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 Opto Std test cell with stand fully equipped for use in both 2 electrode and 3 electrode reference configuration in aprotic electrolytes ECC1 00 0150 A 2 ECC Opto cell cable ECE1 00 0075 A EL CELL User Manual ECC Opto Std Release 2 3 Page 7 of 19 Accessories Kit ECC1 00 0306 A 1 Glass windows 5 pieces LAB0018 V 2 Glass fiber separators 5 pieces ECC1 01 0012 J V 3 Feed wire assy ECC1 00 0010 F 4 Current collector mesh Copper 5 pieces ECC1 00 0328 A V 5 Current collector mesh Aluminium 5 pieces ECC1 00 0328 B V 6 Filling tube with syringe 5 ml for vacuum filling ECC1 01 0001 A 7 O Ring 6 75 mm x 1 78 mm DIC9013 8 O Ring 16 mm x 1 8 mm DIC9012 9 Allen wrench 0 9 mm WZG9005 10 Spherical allen screw driver 3 mm WZG9002 EL CELL ECC1 00 0010 F 1 Feed wire assy ECC Opto 1 pe EL CELL na a l D1C9013 2 EL CELL O Ring 6 75 x 178 pes ECC1 01 0001 A 1pc Filling tube for ECC series d EL CELL Co LAB0018 V 5 pcs Glass disc 22 x 0 3 EL CELL EL CELL 1 00 0328 A V Spcs Current Collector mesh icu a E x18 x P s l T A EL CELL ECCi 01 0012 1 pe EL i Slass fiber separ
5. 328 B gt E WE gt SS S arh D ee ee ft TeSe 7s lest 7 Current collector mesh foil Cu See ECC1 00 0328 A a i OO Glass fiber separator w tong 10 x 1 0 mm ECC1 01 0012 J CE O Ring 16 x 1 8 mm DIC9012 Cell base ECC1 00 0124 A Stand ECC Opto Std FCC1 00 0151 A Feed wire ECC1 00 0010 F Reference electrode ECC1 00 0010 G Compression spring Au FED9015 Plug ECC1 00 0130 B Touch screw ECC1 00 0128 A Piston ECC1 00 0126 A EL CELL User Manual ECC Opto Std Release 2 3 Page 17 of 19 Spare Parts ECC Opto Std ECC1 00 0150 A Stand ECC Opto Std ECC1 00 0151 A ECC Opto cell cable ECE1 00 0075 A Foot for stand VOR9031 Socket screw Lid DIN 912 M4x10 Lid ECC1 00 0127 A Cell base ECC1 00 0124 A Feed wire ECC1 00 0010 F Compression spring 10 N Au standard 5 pieces FED9015 V Spring forces see page 12 Compression spring 20 N Au 5 pieces FED9020 V Spring forces see page 12 Compression spring 30 N Au 5 pieces FED9021 V Spring forces see page 12 Touch screw ECC1 00 0128 A Reference electrode pin ECC1 00 0010 G Plug ECC1 00 0130 B Piston ECC1 00 0126 A Accessories Kit ECC1 00 0306 A Feed wire assy ECC1 00 0010 F Filling tube with syringe 5 ml for vacuum filling ECC1 01 0001 A Allen wrench 0 9 mm WZG9005 Spherical allen screw driver 3 mm W2ZG9002 EL CELL User Manual ECC Opto Std Relea
6. 6 10 Warranty a oiaaereerctt streetscene tune ntunnde aotapenentan eacnemneaeeminesenanaeseiaanansesensaaneie 16 Appendix Components ECC Opto Stl 2 0 cccccc cece s eee e eens senna esas ene ee eaeenaeeeeaetnasenaeeteaees 17 SD AFG PACES sescccncscnesecciwectapsscontstetnastadudceniadetansteieiceniaestansteteiessiabsianieceedaseteietuesdecs 18 Consum DIGS 555 2cccncieecaccsctacansassaice nies aseesineed tieienncssusasimenncaaiavoncasemusanecimeadnasnaunee 19 EL CELL User Manual ECC Opto Std Release 2 3 Page 3 of 19 1 Product Description 7 Cell body Port C Reference pin CE Port B Electrolyte filling port Port A Contact pin WE Touch screw The ECC Opto Std test cell serves to monitor the optical properties of an electrode material in the course of electrochemical charging For this purpose the working electrode WE material which is supported on a meshed or holed current collector is placed right below the optical window This WE is sandwiched from below with a glass fiber separator and an appropriate counter electrode CE This way the optical instrument looks from the top through the optical window onto the backside of the electrode material WE Typical instrumentations include optical microscopy and confocal Raman spectroscopy in the reflection mode A re fitting kit for X ray is avail
7. EL CEEL electrochemical test equipment User Manual Release 2 3 Electrochemical Test Cell ECC Opto Std 22 June 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 ECC Opto Std Release 2 3 Page 2 of 19 Content 1 Product DESGCFI DUO W iiidciisciiicciicsisctctnstaasadssdanisdandasaiaasdiscadsadataaiassasinaatsaniadaniann 4 7 ae gO eee eee 6 3 Safety Prec3UtiONS crino Sau toontoenccaencenmoeneds 7 4 Unpacking sssesesssnsssnsrsnnnnnrrrrnnnnnnnnrrnnnnnnnnnnnrnnunnnnnnrnrennnnnnnrnrrunnnnnnnrrrnnn nnne 7 5 Assembly and Connection sssssssnnnnrrrrrrrssssssssnnnnnnnnnnnnnnnrrrrrrrrrereeennnnne 9 6 Disassembly and Cleaning cccccccceccceee eee esse eeeeeeeeeeeaee ease eaeeeaeeeaaeeeaees 12 7 X Ray EXperime nts cccccececeeceeeceeeeseeeeeseeeeseeeesgeeeegeeeeeaeeeegenetsaeetegenetsaners 13 CURE TS soccer AEAEE EAE E AAR 15 9 east SUPPO E e A 1
8. able as an option view page 13 The maximum diameter of the working electrode WE is 10 mm while that of the inspection hole is 1 mm optional up to 10 mm The cell is equipped with a reference electrode pin for 3 electrode operation EL CELL User Manual ECC Opto Std Release 2 3 Page 4 of 19 Functional principle of the ECC Opto Std Inspection area 1 mm optional up to 10 mm Working electrode material WE placed on the current Optical window collector mesh Current collector mesh Aluminium or Copper 16 mm Spring loaded piston Glass fiber separator Counter electrode CE a ae ee E S Reference electrode pin Q S Detend feature Working electrode contact pin EL CELL User Manual ECC Opto Std Release 2 3 Page 5 of 19 2 Features 2 and 3 electrode cell with optical window for aprotic electrochemistry Materials in media contact are stainless steel 1 4404 PEEK and EPDM The backside of the working electrode material can be observed through sthe optical window on top Inspection area diameter is 1 mm Other diameters up to 10 mm available Typically used in combination with optical or Raman microscopy in the reflection mode X ray option with Beryllium window available The window is made of optical glass Sapphire Beryllium and Kapton windows are available on request Working electrodes can be single crystals or grains powder samples and boun
9. ator wen tongue 10x1 i CELL EL CELL ECC1 00 0328 B y 5 pes W2ZG9005 Current Collector mesh AL i H Allen wrench 0 9 mm p JA EL CELL User Manual ECC Opto Std Release 2 3 Page 8 of 19 5 Assembly and Connection Generally all assembly steps are to be carried out in inert glove box atmosphere All components used are to be dried upfront in a vacuum oven at 80 C for at least 12 hours Once fully assembled the cell is hermetically sealed so that it may be operated in ambient atmosphere The test cell can be used in either 2 electrode or 3 electrode reference configuration In the following the cell assembly is described for operation with graphite powder as the working electrode and lithium metal reference electrode Assembly 1 10 11 12 By means of the optionally available ECC RefLoad press a small piece of lithium metal into port C so that the Lithium metal just appears at the upper narrow end of the feed through hole Skip this initial step if working without reference electrode Push the counter electrode piston into the cell body to the uppermost position Pull the piston slightly back and insert the Lithium counter electrode max 10 mm in diameter max 1 mm thick Put the provided glass fiber separator on top Place a small amount a few milligrams of graphite powder onto the center of the separator An ionizing device helps to prevent the build up of electrostatic excess charge
10. d electrodes applied onto current collector mesh Maximum electrode diameter is 10 mm Easy and clean electrolyte filling via the vacuum syringe method All necessary equipment is included Cell assembly and filling are to be carried out inside a glove box Once sealed the cell may be operated outside the box at ambient atmosphere Small and defined electrolyte volume down to 0 1 cm due to minimized dead volume Connection to potentiostat battery tester via 2 mm banana sockets adapters for 4 mm banana sockets are included Temperature operation range 20 to 70 C Dimensions of the ECC Opto Std mm EL CELL User Manual ECC Opto Std Release 2 3 Page 6 of 19 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 X ray option view page 13 Beryllium is highly toxic and can cause cancer Take proper precautions when handling the Beryllium window Avoid direct contact with skin Carefully collect and dispose properly any Beryllium fragments when accidentally breaking the window 4 Unpacking Check the contents of the
11. e 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 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 ECC Opto Std Release 2 3 Page 16 of 19 Components ECC Opto Std Socket screw DIN 912 M4x10 Lid ECC1 00 0127 A Glass window 22 x 0 3 mm LAB0018 Current collector mesh foil Al pe ECC1 00 0
12. se 2 3 Page 18 of 19 Consumables Accessories Kit ECC1 00 0306 A Glass window 5 pieces LAB0018 V Glass fiber separator 5 pieces ECC1 01 0012 3 V Current collector mesh Copper 5 pieces ECC1 00 0328 A V Current collector mesh Aluminium 5 pieces ECC1 00 0328 B V O Ring 6 75 mm x 1 78 mm DIC9013 O Ring 16 mm x 1 8 mm DIC9012 EL CELL User Manual ECC Opto Std Release 2 3 Page 19 of 19
13. steps to complete filling Remove the filling tube and close port B with the second WE contact pin 13 Insert the cell into the stand EL CELL User Manual ECC Opto Std Release 2 3 Page 10 of 19 14 Connect the cell to the cell cable as shown in the picture below 15 Connect your potentiostat to the 2 mm sockets 1 of the cell cable grey REF red WE blue CE Adapters 2 are provided for connection to 4 mm banana sockets EL CELL User Manual ECC Opto Std Release 2 3 Page 11 of 19 Different spring forces in relation to stack thickness A compression spring exerts the mechanical pressure on the cell stack Different springs with a nominal pressure of 10 20 and 30 N are available The applied pressure slightly depends on the thickness of the cell stack 35 30 FED9015 Standard FED9020 25 FED9021 20 a N 15 10 eS Spring force applied on cell stack N 0 200 400 600 800 1000 Thickness of electrode stack um 6 Disassembly and Cleaning Right after use disassemble the cell in the reverse order of assembly All chemicals used have to be disposed properly All wetted parts are to be cleaned with water and or other appropriate solvents All parts are to be dried immediately after cleaning at 80 C NOTE Leaving cell parts in contact with ambient atmosphere while still being wetted with electrolyte may result in severe corrosion EL CELL User Manual ECC Opto Std Release 2 3 Page 12
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