User Manual - EL-CELL
Contents
1. 2z2222e0 000nn0nnnnnnnnn nun nen nn nun nun RER nn nn nn Rn 25 Using an AUxilary Elect6de un 25 Changing the WE Load cccccsscccssccessecenseceneececsececuecncuscneussneuesneatsneatens 26 Using Single Crystals or Grains as the Working Electrode cccecseceeeeees 27 Using Powder Type Working Electrodes u uu2z0200000n0nnonnnnn ann nn nn nn nn nn 27 Accessories and Spare PartS u2z22s2s2n0nnnnnnnnn anno nn nn nn nn nn nn nun nn nn nn nn ann nn nennen 28 Connector and Cable Pin out z2z02u02002000nnn nn nn nn nn nn nn nn nn nn nnnnnnnnn 35 MaINlENANCE een sahne 37 TECHRICAl SUDO nee 37 Appendix AC Electrode Results ccccsscssssescsreecereecerseccuseecuseeusenesaneesaress 38 YUV ALLE i et nn eee ne 39 Page 3 of 39 EL CELL 1 Product Description The ECD 1 electrochemical dilatometer is dedicated to the measurement of charge induced strain expansion and shrinkage of electrodes down to the sub micrometer range The ECD 1 is 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 films single crystals e g HOPG or binder free powders The maximum electrode size is 10 mm x 1 mm diameter x thickness The heart of the ECD 1 is an electrochemical cell hermetically tight against2. Spring loaded CE plunger hnical Specifications LVDT sensor with two signal outputs 2 to 10 V and 10 to 10V and selectable gain Signal conditioning for connection to a data logger and or to the analog input channels of the controlling potentiostat battery tester Measurement range of 500 um Resolution of lt 50 nm Drift stability of lt 100 nm hour sample free instrument at constant temperature Sample working electrode bound film binder free powder or single crystal grain max sample size 10 mm x 1 mm diameter x thickness Load on working electrode 0 3 N or 1 3 N Electrolyte volume lt 3 ml Materials in contact with electrolyte PEEK borosilicate glass EPDM rubber and stainless steel 316L for aprotic gold for aqueous electrolytes Operating temperature range Cell and Sensor 20 to 70 C Controller and Data Acquisition System 0 to 40 C EL CELL Minimum dimensions for glove box ante chamber transfer stand detached Dimensions ECD 1 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 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 anyt
3. 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
4. 102 Shunt Voltage DC Voltage Auto 6 5 Moe DJ 1 D YDE 103 Cell Voltage 1 vs 2 DC Voltage Auto 55 More DJ 1 D YDE 104 WE Potential 1 vs REF DC Voltage Auto 55 More DJ 1 D YDE 105 CE Potential 2 vs REF DC Voltage Auto 55 Moe O 1 D YDE 106 O AU Potential SU ws REF DC Voltage Auto 5 5 More O 1 0 YDC 107 Temperature Temp 4 ire ATD Hone C Moe 1 1 D E 108 O Sensor Voltage 2 DC Voltage Auto 6 5 More O 1 D YDE 109 O DC Voltage Auto 55 l O 1 0 YOC 110 O DC Voltage Auto 5 5 O 1 0 YOC 111 O DE Yoltage Auto 5 5 MW 0 YOC 112 O DC Voltage Auto 5 5 O 1 0 DE 113 O DC Voltage Auto 5 5 O 1 O DE 114 O DC Voltage Auto 5 5 O 1 O DE 115 O DC Voltage Auto 5 5 MW i DE 116 O DC Voltage Auto 55 l O 1 0 YOC 117 O Temperature Temp 4 ire ATD Hone E More J 11 0 C 118 O DOC Voltage Auto 55 O 1 0 WDC 113 O DOC Voltage Auto ans O 1 0 YDC 120 O DC Voltage Auto 5 5 E D YDE 121 O DC Current Auto 5 5 O 1 D ADC 122 O DC Current Auto 5 5 O 1 D ADC Computed Channel 901 Displacement Multiply 101 1 0 00012025 0 ha 902 Cell Current Multiply 102 1 0 01 0 ADC Add set up the data logger s channel list according to the screenshot given above For software installation and data logger operation refer to the separate instructions coming along with the data logger For best precision set the resolution of channels 101 102 and 107 117 to 6 5 digits 10 NPLC Notice the impact of the resolution chosen and the number of channels activated on the
5. It has a fixed bandwidth of 300 Hz 3 dB and a fixed gain of Ah AV 0 00012025 m V 120 25 um V S N calibration date The gain and bandwidth of V2 are selectable by the DIP switches at the controller box ON ON anav x25 481umV ON OFF AWAVax5 24 05 m V OFF OFF anav x1o 12 025 um V Switch 3 Switch 4 Bandwith V 3 dB ON 300 Hz OFF The bar graph LED display at the controller box refers to the second displacement signal V2 at the actually chosen gain The center of the bar graph display corresponds to an analog output signal V2 of around OV the outermost red LEDs indicate that V2 is outside the valid range of 10 to 10V The signal V2 is available to the data logger potentiostat via the Sub D data logger connector and at the BNC connector 5 3 Recording the displacement signal with the data logger The standard version of the ECD 1 comes with the Agilent 34970A data logger and the associated Benchlink software application The data logger has to be configured to record the displacement signal along with the cell current the electrode potentials and the temperature inside the chamber Configure Instruments Configure Channels Scan and Log Data Schnelldiagramm Channek Enable Channel Measurement Scaling Mx E r Instrument Scan Mame Function Range Res More Scale Gain M Offset B Label 1 Not Connected 349014 101 Sensor Yoltage 1 DC Voltage Auto 65 Moe 0O 1 D VOC
6. Release the sensor plunger and fix it again By doing so the bias load resulting from the flexure deflection is reset to zero Page 17 of 39 Connect the instrument via the cell and sensor cables to the controller box Page 18 of 39 ECD 1_manual 2012 02 02 02 02 2012 z F 5 2 Connecting the Instrument Sensor Cable Cell Cable Controller T Chamber X connection to potentiostat optional Data Aquisition System 1 Place the ECD 1 inside a temperature controlled chamber at a constant temperature between 20 to 70 C 2 Establish all electrical connections between dilatometer controller and data logger according to the diagram given above 3 Connect your potentiostat or battery tester to the 4 mm jacks on the front panel of the controller box Refer to the table given below Controller Box Potentiostat 2 CE Page 19 of 39 EL CELL 4 Connect the 2mm banana plugs of the cell cable to the dilatometer cell Refer to the photo on page 19 The displacement signal can be recorded via the data logger or if available by an analog input of the potentiostat that is used for charging the electrochemical cell It is also possible to record the displacement signal simultaneously on both the data logger and the potentiostat Two analog signals are provided one in the range 2 to 10V the other one in the extended range 10 to 10V V is only available at the Sub D data logger connector
7. ambient atmosphere The two electrodes inside are separated by a stiff glass frit that is fixed in position The upper working electrode is sealed by means of a thin metal membrane 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 WE without any interference from that of the counter electrode CE N LVDT sensor membrane fe REF A high resolution displacement LVDT transducer a acts dimensional changes of the WE ranging from 50 nanometers up to 500 micrometers during one and the Same experiment that may last between a few minutes to many days A simple weight serves to adjust the load on the working electrode For best accuracy and drift stability we recommend operating the ECD 1 inside a temperature controlled chamber This manual covers the ECD 1 Standard version together with the optionally available re fitting kit for aqueous electrolytes Page 4 of 39 EL CELL Exchangeable weight control load on WE Spacer disc for height Valve assembly for vacuum filling adjustment via syringe to Metal membrane Auxiliary Glass T frit separates WE test specimen on top from CE below 2 Tec Page 5 of 39 Friction free flexure guide Sensor plunger port Reference electrode assembly Gas filled dead volume to suppress changes in hydrostatic pressure inside cell
8. current collector disc on top of the CE NOTE For aprotic organic electrolytes this disc is not required gt 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 39 6 Stack cell bottom with central CE piston inserted on top Put base fle top hold the around Screw the assembly tog hex socket screws M4x25 ECD 1_manual 2012 02 02 02 02 2012 Attach the ce the two knurle 10 Screw in the uppermost positi turning the scr w bac Put the WE or with the active Page 11 of 39 ECD 1_manual 2012 02 02 02 02 2012 EL CELL 12 Place the spac aqueous stainless electrolytes C ontop of de WE gold for teel 13 16L for NOTE By using the 2 1 mm thick spacer disc the neutral flat position of the membrane corresponds to an initial working electrode thickness of 250 um see sketch Height changes between 250 and 250 um relative to the neutral position are acceptable without causing excessive bending of the membrane WE Spacer disc Metal membrane CE Page 12 of 39 EL CELL Place the co ve Page 13 of 39 ECD 1_manual 2012 02 02 02 02 2012 Fasten the cove socket screws M4x3 17 Interconnect cell v tubings as indicated by the numbering on the parts 18 Close the side opening
9. maximum scanning speed of the data logger At optimum precision and when all channels in the scan list are check marked the scanning speed is limited to approximately 0 5 Hz 2 seconds each scan Channel 102 902 To record the cell current the voltage drop across a 100 Ohm resistor looped into the CE supply line is fed to channel 102 The 100 Ohm 1 Watt 1 resistor is located inside the controller box and is protected against overload by a 100 mA fuse Both the resistor and the fuse can be replaced as necessary For convenience add two computed channels to the data logger s scan list in order to directly display the electrode displacement in meters and the cell current in Amperes Refer to the two computed channels at the bottom of the scan list shown above Page 21 of 39 EL CELL Channels 107 117 These two channels are configured to measure the temperature by means of a 4 wire Pt100 sensor that is located inside the cell cable terminal close to the dilatometer 5 4 Recording the displacement signal with a potentiostat optional Many battery testers and potentiostats provide additional analog input channels that may be used to record the displacement signal along with cell current and potential In the following connection of the ECD 1 to the Biologic VMP3 is described Adaption to many other potentiostats is possible as well I Connect the 9 pin Sub D connector of the data logger cable to the analog input of the respective VMP
10. single crystal wE ECD1 00 0008 B CE Spring Load II H FCD1 00 0005 B Central CE Piston II aprotic 1 4404 oP ECD1 00 0006 B Central CE Piston Il aqueous ene aaa OS fernen am m ECD 1 00 0013 A Part Kit Flexure Unit ECD1 00 0015 A Part Kit Screws ECD1 00 0017 B Part Kit Springs Il De ECD1 00 0016 A Part Kit Tubings Br n ECD1 00 0010 B Reference Electrode aqueous UNF 1 4 28 Reference Electrode aprotic ECD1 00 0009 B UNF1 4 28 1 4430 Oo ECC1 00 0018 B 2mm spacer disk aprotic aaa Oo ECC1 00 0018 A 2 mm spacer disk aqueous BT Terminal board with 2nd Data Socket Screw M4x30 part N_912 Cover Flange part ECC1 00 0016 B Socket Screw M4x25 part N_912 Spacer Disc aqueous part ECC1 00 0018 A spacer disc aprotic part ECC1 00 0018 B PTFE Plug 1 4 28 part LABOOOS Cell Body part ECC1 00 0015 C Ferrule 1 16 part LABOOO2 Nut flangeless 1 6 in 14 28 part LABOOO1 Ferrule 1 16 Cell II assy part ECD1 00 0002 B Membrane aqueous part ECC1 00 0019 A Nut flangeless 1 6 in 14 28 part LABOOO1 Ferrule 1 16 part LABOOO2 WE O Ring 33 05x1 78 part DIC9005 T Frit part ECC1 00 0041 A CE Current Collector part ECC1 00 0033 A only aqueous Cog part LABOOO2 Cell Bottom REF Electrode II aqueous part ECD1 00 0010 B part ECC1 00 0011 B Central CE Piston aqueou
11. terminated with 2 mm banana connectors to ECD 1 cell Color of 2mm Pin Signal Cable Color Connector 1 vi Red red c ee 6l AUX Pik black 7 S S 8 5V_ whiteyblue ee ee E BEE T HE d S Data Logger Cable 8x2 TP shielded One end of the cable is terminated by a Sub D HD F15 connector to box the other end is terminated by the multiplexer card of the data logger am Red Hanns RB Whtegreen yon BEE EEE BEE 1 ee Analog Output Cable 4x1 shielded Optionally the datalogger cable is split into a second cable that is terminated with a Sub D M9 connector This connector fits directly into the auxiliary input connector of the Biologic VMP3 potentiostat Adaption to other second party instrumentation is available on request ni Color VMP3 AUX connector mei Sensor Signal V green Analog IN1 N se 6 Sensor Signal V gt Analog IN2 Sensor Cable SUB D F15 to box Round connector to sensor Ba secondary white we secondary brown BE S ae 3 mid grey Caa a EEE 6 primary black U a aa 8 Maintenance Right after finishing an experiment disassemble the instrument dispose the electrodes and clean all parts that have been in contact with electrolyte Depending on the electrolyte and electrodes used the wetted parts may be cleaned with water dilute detergent wash ethanol or acetone Ultrasonic cleaning is recommended Tubes and valves are to be purged with the
12. 3 channel Il Edit the cell characteristics settings of the VMP3 channel so as to record either one or both of the two analog inputs Analog IN1 is connected to the displacement signal V4 with fixed gain Analog IN2 to the displacement signal V2 with variable gain Record I Eces Screenshot from the Biologic EC Lab Software z ee showing the analog input configuration I Analog IN 17 Analog IN 2 Record external devices an Analog IHH WE ref Ea refs CE External Devices RDE Configuration x Channel Device Type Device Name fi Other Other CONTROL MEASURE Analog OUT Analog IM 1 Convert TAC to ev If Convert EAM Displacement um with 100 IL mas 240 5 um ma 0 ale fo W min Manual Contro 240 5 rn mir TAC 60 Convert EM to Displacement um with fio Y 120 25 am max 5 0 YW 5 20 25 rn mir Custom Variables OF Cancel Apply Page 22 of 39 EL CELL NOTE Before starting the electrochemical cycle we recommend holding the cell at open circuit for several hours to allow for baseline stabilization Following this procedure helps to discern charging induced dimensional changes from creeping Note that all materials display a more or less pronounced creeping They tend to shrink after applying a load and to swell when removing this load Creeping of the working electrode is initially induced when applying the load It is also induced each time the
13. EL CELL electrochemical test equipment Electrochemical Dilatometer ECD 1 User Manual Serial No Release 2 2 2007 2012 2012 02 02 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 6 D 21079 Hamburg Germany phone 49 0 40 790 12 733 fax 49 0 40 790 12 736 info el cell com Page 2 of 39 EL CELL Contents KR W N e 5 2 5 3 5 4 5 5 5 6 5 7 5 8 5 9 5 10 5 11 10 11 Product DOSCAN van 4 Tecnnical SpeciNCaUONS ee en 5 Safety PFECAUTIONS anne 6 UNPACKING PREPEEREENERFEIFEPERFEEEIEEEFEREFVERFERENFERFEEETPENEEEENEREENEEPENFEERIEEEREREIUEEEERENEERERER 6 EC ODO TUON nenne 8 ASSEIMIDIY ororen eoero E EEEE ORNER 8 Connecting the INStruMent scccsscccssecessccecsccecuececuscecuscueuscneussneursnearens 19 Recording the displacement signal with the data logger ccceeeeeeeeees 21 Recording the displacement signal with the potentiostat Optional 22 Sensor Sleeve Adjustment ccccsccecsececsecncuecncuecneuronearsuearsueceneeseneeseseess 23 ECDs DISasse DV een ae 24 Using the Reference Electrode
14. NOTE Optionally this auxiliary electrode Page 14 of 39 ECD 1_manual 2012 02 02 02 02 2012 EL CELL ale Attach the reference ele for aqueous SS pin for a NOTE The ence pi appropriat J l d with the a material Dead volume valve re Syringe valve yellow lyte according to the L 1 Charge a 20 ml syringe with ca 3 ml of electrolyte We recommend one time use PP plastic syringes with low friction polysiloxane pistons Fill the cell with elect following proce 2 Connect the syringe to the Luer adapter of the inner syringe valve 3 Open the syringe valve and close the outer dead volume valve 4 Pull the syringe piston back to evacuate the cell Hold the piston a few seconds in the strained position 5 Release the piston so that the electrolyte is drawn into the cell 6 Repeat the two previous steps to complete filling 7 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 39 EL CELL Page 16 of 39 21 Attach the sensor loa flexure guide locked 22 Fasten the sensc oa socket screws M4 unit y means of the 3 hex Unlock the flexure guide to lower the sensor tip down to the membrane ese evn amp
15. Page 31 of 39 EL CELL 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 LABO007 Page 32 of 39 EL CELL CE Spring Load II part ECD1 00 0008 B Spring 1 0x10x26 Spring Ram II part FED9015 part ECC1 00 0022 C O Ring 15 6x1 78 Adjusting Screw part DIC9008 part ECC1 00 0021 B Reference Electrode II aqueous part ECD1 00 0010 B Reference Electrode II aprotic part ECD1 00 0009 B Ref Electrode II a ae part ECC1 00 0062 B Fitting 1 7mm Reference Electrode Ae apres part ECC1 00 0039 C part ECC1 00 0062 Set Screw M2x2 part N_916_M2x2 Spr Er met Hollow Screw Set Collar 1 O Ring 1 5x2 part ECC1 00 0040 A part ECC1 foo 0038 C part DIC9007 Sensor Load part ECD1 00 0011 A Part Kit Load ne ECD1 00 0007 A part ECC1 00 0025 A LVDT Sensor part SEN9018 Sensor Plunger M2 part ECC1 00 0017 C Set Screw M3x4 part N_913 Gauge Tip Ruby part VOR9014 7 Connector and Cable Pin out Cell Cable 8 x 2 TP shielded One end of the cable is terminated with a Sub D HD M15 connector to box the other end is
16. 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 6 Fitting 1 7mm 7 O Ring 1 5x2 3 Set Screw M2x2 4 Spring A t ar 5 Hollow Screw 2 Set Collar 1 7 1 Reference Pin 5 8 Using an Auxiliary Electrode As an option the ECD 1 may be equipped with an additional electrode face to face with the 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 simulta
17. aid of a syringe Right after cleaning all parts have to be dried in vacuum at max 80 C Check O ring seals and the T frit visually for damage and replace as necessary 9 Technical Support Technical support for this product is exclusively handled by EL Cell GmbH The following procedure must be followed when the ECD 1 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 D Return the instrument to EL Cell GmbH Tempowerkring 6 D 21079 Hamburg Germany Email info el cell com Page 37 of 39 EL CELL 10 Appendix AC Electrode Results The ECD 1 comes with a set of activated carbon AC double layer electrodes 0 2mm thick and 9 mm in diameter These electrodes may be used to get quickly familiar with the test procedure The electrodes contain 75 wt of a mesoporous activated carbon with 1200 m g surface area BET and 25 of PTFE as a binder The following diagrams show the dilatometric response of this electrode material during the first 10 cycles in 1 2M LiPFg in EC EMC 3 7 with a scan rate of 5 mV s between 3 0 and 1 5V vs Li Li Lithium metal was used as both the counte
18. hing is missing or damaged NOTE Damaged shipments must remain with the original packaging for freight company inspection Page 6 of 39 EL CELL List of Components Standard Version 1 eS a ECD 1 dilatometer in the assembled state equipped for use with aprotic electrolytes Signal conditioning electronics controller box with DC power supply Cell cable sensor Cable Data logger cable Agilent 34972A Data Acquisition System Data Logger with 34901A 20 channel multiplexer board 34825A Benchlink Data Logger Software and documentation drivers on CD 20 ml syringe with polysiloxane sealing Vacuum pipette and tweezers for electrode handling Hex wrenches for assembly and maintenance 3 tubing assemblies for interconnection between cell valves and syringe Activated carbon electrode set 5 pcs for reference measurements Re fitting kit for aqueous electrolytes to be ordered separately Page 7 of 39 EL CELL 5 ECD 1 Operation 9 1 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 39 EL CELL Page 9 of 39 3 Place CE dia lt 20 mm with the active layer downside on top of the glass frit 4 Place
19. mechanical properties of the working electrode are significantly altered by charging Therefore each charging induced height change is followed by some creeping Both the initial and the charging induced creeping effects are real and not artefacts of the measurement 5 5 Sensor Sleeve Adjustment For optimal utilization of the displacement range for very thick samples or for samples showing large expansion it may be advantageous to alter the mechanical null position of the sensor This is to be done on the fully assembled instrument Release the hex socket screw 1 and move the sensor sleeve 2 vertically into the desired position Significant force is to be applied to move turn the sleeve The corresponding sensor signal on channel 101 must be between 2 and 10 V referring to the upmost and lowermost valid position of the sensor sleeve Fix the sleeve at a sensor voltage of about 6 V to start the measurement at mid range Note The valid adjustment range is about 0 5 mm relative to the default position of the sensor sleeve Outside this range the sensor signal is no longer linearly related to displacement The sleeve may be lowered by approximately 5 mm before collision with the plunger core inside Avoid collision in any case 2 5 6 ECD 1 Disassembly 8 9 Open the potentiostat s charging circuit and unplug the power supply from the controller box Disconnect all cables from the dilatometer Then remove the instru
20. ment from the temperature chamber Lock the flexure guide in the upper position by moving the adjustment wedge into the leftmost position Detach the sensor load unit Remove the plug from the cell body and open the syringe valve Then draw any free electrolyte back into the syringe and close the syringe valve Detach the reference electrode Disconnect all tubings from the valves and from the cell Remove the cover flange the metal membrane the spacer disc and the working electrode NOTE The membrane may be re used many times A slight bending and a tiny dent in the center of the membrane are normal signs of use Unscrew the counter electrode spring load Detach the remaining cell from the bracket 10 Unfasten the cell body and remove the T frit from the cell body NOTE Take care not to jam or break the frit The frit may accidentally slip out of the cell body 11 Clean all parts that have been in contact with electrolyte Depending on the electrolyte and electrodes used the wetted parts may be cleaned with water dilute detergent wash ethanol or acetone Ultrasonic cleaning is recommended Dry all parts immediately after cleaning in vacuum at 80 C overnight It is highly recommended to additionally dry cell body and cell bottom in vacuum at 150 C overnight Absorbed moisture may otherwise adversely affect test results Check O ring seals and the T frit visually for damage and replace as necessary 5 Using the
21. neously 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 5 9 Changing the WE Load By default the sensor load unit is equipped with a weight appr 100 g to assure a good electrical contact between the working electrode and the membrane over the whole displacement range In some situations however it may be preferable to apply only the dead load of the sensor plunger and the flexure ca 30 g in the neutral position To remove the 100 g weight follow the instructions given below 1 Detach the sensor load unit from the dilatometer cell 2 Release the knurled screw 1 3 Pull out the sensor plunger 4 with the weight 2 attached on it 4 Release the set screw of the weight with the provided hex wrench 3 and remove the weight Insert the plunger 4 into the leftmost position and fasten the knurled screw 1 Attach the sensor load unit back to the cell Unlock the flexure guide Release the knurled screw and re fasten it thereby moving the flexure guide in its neutral position Make sure that the sensor tip 5 is sitting on the membrane ON Dw Knurled Screw 1 Weight 2 Hex Wrench 3 Sensor Plunger 4 Sensor Tip 5 5 10 Using Single Crystals or Grains as the Working Electrode As an option the ECD 1 may be loaded with a single crystal o
22. r and the reference electrode Similar results are obtained with other common Li ion battery electrolytes 40 35 30 25 20 1 um AHeight um 5 400 sec ml mA 3 0 2 5 2 0 1 5 Eu V 0 2000 4000 6000 8000 Time s 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 Sellers 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
23. r grain as the working electrode For this purpose the ball tip of the sensor load unit is to be replaced by a flat tip and the membrane is directly placed on top of the crystal without the spacer disc in between More detailed instructions come with the optionally available Part Kit for Single Crystals 9 11 Using Powder T ype Working Electrodes The ECD 1 is also capable of using binder free powders as the working electrode Simply place a separator on top of the glass frit to prevent contamination of the frit and subsequently a small amount of the powder appr 5 to 15 mg Just as for the measurements of single grains cover the sample directly with the metal membrane and use the sensor load unit equipped with the flat tip Part kit for Single Crystals Filling the cell by the syringe vacuum technique prevents that loose powder is flushed away during the filling procedure NOTE Make sure that the sample has sufficient electronic conductivity and that the contact resistance between sample and membrane is tolerable An additional interlayer e g gold foil for aqueous carbon coated aluminium or copper foil for aprotic electrolytes between sample and membrane may reduce the contact resistance drastically Page 27 of 39 EL CELL 6 Accessories and Spare Parts cam ECC1 00 0019 C membrane aprotic a a ECD1 00 0014 A Part Kit Sealings ee sinter eo ECC1 00 0041 A T Frit 20 10 glass poros 3 5 ECD1 00 0018 A Part Kit for
24. s part ECD1 00 0006 A Central CE Piston aprotic part ECD1 00 0005 A Base Flange part ECC1 00 0014 A REF Electrode II aprotic part ECD1 00 0009 B O Ring 21 95x1 78 part DIC9003 O Ring 41x1 78 part DIC9001 Valve Support assy CE Spring Load part ECD1 00 0008 A Page 29 of 39 part ECD1 00 0004 A Countersunk Screw M3x8 part N_7991 EL CELL Valve Support II assy part ECD1 00 0004 B Thread Rod Cap Nut M3 part ECC1 00 0052 A part N_1587 Female Luer to 14 28 Male part LABOOO6 Shut Off Valve 1 4 28 yellow part LABOO11 Valve Support part ECC1 00 0035 B Syringe Ferrule 1 16 part LABOOOS part men A Spacer A part ECC1 00 0050 A Nut 1 6 1 4 28 part LABOOO1 part LABOOO2 Shut Off Valve 1 4 28 red part LABOO10 Nut 1 6 1 4 28 part LABOOO1 _ Cap Nut M3 part N_1587 Ferrule 1 16 part LABOOO2 Sensor Load unit II part ECD1 00 0012 B Clamp Sleeve Socket Screw M4x30 part ECC1 00 0027 A part N_912 Part Kit Socket Screw M4x12 ECD1 00 0013 A part N_912 Sensor Support part ECC1 00 0026 A Sensor Fixure part ECC1 00 0013 D Flexure part ECC1 00 0012 A Socket Screw M3x10 part N_912 Adjustment Wedge II part ECC1 00 0031 C Knurled Screw M2 6 part ECC1 00 0051 A Sensor Load part ECD1 00 0011 A Knurled Screw M4x16 part SON9004
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