Combined EIS- and Spectro-Electrochemical Absorbance Measurement Experiment. Practical Course 2 C.-A. Schiller

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1 Combined EIS- and Spectro-Electrochemical Absorbance Measurement Experiment Practical Course 2 C.-A. Schiller Kronach Impedance Days 212

2 KIT 212 CIMPS-abs 1 Introduction Classical optical absorption spectroscopy OAS is a well established technique since many decades. OAS is defined by a continuous spectral record of an objects optical absorption over a moderate to wide range of wavelengths in the UV, VIS or IR light. It is very important for mechanistic and structural chemistry and a standard in analytical chemistry. The full strength of OAS is displayed in combination with further supporting techniques. The set-up for the fields of electrochemistry uses a wideband light source like a tungsten lamp to illuminate a transparent electrochemical cell (Photo Electrochemical Cell PECC ) and the transmitted light is analyzed by means of a spectrometer. Following this idea, Zahner developed CIMPS-abs in order to combine light absorption spectroscopy and general spectro-electrochemical measurements with standard electrochemical techniques like potentiostatic and galvanostatic polarization, CV-sweep and dynamic techniques like impedance spectroscopy. High precision spectroscopy is enabled by means of an electro-mechanical slide, which supports the automatic change between the measurement cell and a reference cell in the optical path between light source and spectrometer head. Besides of manually triggered spectra, automatic series of absorption spectra in dependency of electrochemical parameters can be run in single sweep, cyclic, or vs. time mode. In addition to it there is a really cunning feature of the CIMPS-abs software: automatic series measurement of absorption spectra can be combined with a user defined script. Such a script may provide prescriptions for procedures which are executed before and after each absorption spectrum. By this for instance automatic electrochemical pre-treatment for each optical spectrum can be organized or automatic EIS spectra can be combined with the optical characterization during an electrochemical sweep. impedance / Ω.6-1 mv 1K mv 3K extinction mv +75 mv 1K 3K 1K +35 mv mv mv wavelength / nm 3 1m K 3K 1K frequency / Hz Fig. 1: A typical application example for CIMPS-abs: Extinction spectra series vs. cell voltage referenced to Ag/AgCl 3m-NaCl of a P3HT-PEDOT:PSS film in Acetonitrile / TBA-PF 6 (left hand side) and the corresponding impedance spectra (right hand side).

3 KIT 212 CIMPS-abs 2 The Aim of the Experiment The combination of mixed DC-pre-treatment-, optical absorbance- and impedance spectra recording in an automatic measurement SER set-up shall be understood on the example of a polymer film model system for Organic Solar Cell and Organic LED. Fig. 2: Band schemes of a typical OSC (bulk hetero-junction type, left) and an OLED (three layer type, right). p: hole transport layer (e.g. PEDOT:PSS), n: electron transport layer (e.g. left: PCBM as e - -acceptor. right: Alq 3 [tris(8-hydroxyquinoline) aluminium]), BG: active band-gap material for photon absorption (left, e.g. P3HT as e - - donor) respectively electron-hole recombination under light emission (right, e.g. Ir(ppy) 3 = fac tris(2- phenylpyridine) iridium). Fig. 2 sketches the two most important applications of photo-sensitive organic polymer films: OSC and OLED. The sample in the experiment is a multilayer similar to a part (left hand = anodic side in Fig. 2 left) of an OSC. Fig. 3 shows the details of the multilayer sample inside the Photo-Electrochemical Cell PECC. It starts with a transparent conducting oxide TCO on a glass carrier. The next layer is the hole transport layer PEDOT:PSS, what is a mixed polymer from Poly(3,4-ethylenedioxythiophene) poly(styrenesulfonate), a transparent p-semiconductor with a relatively high electrical conductance. Fig. 3: Section scheme of the measurement sample (not to scale) in the photo-electrochemical cell PECC2 (left) and the PECC2 picture (right). PEDOT:PSS: 17 nm hole transport layer, P3HT: 13 nm active band-gap material for photon absorption, applied by successive spin coating from aqueous (PEDOT) and non-aqueous (P3HT) solution. Area: 3.2 cm 2. Layer annealed at 11 C, 4h, N 2. Electrolyte volume kept under N 2.

4 KIT 212 CIMPS-abs 3 The photo-active material is a film from Poly(3-hexylthiophen-2,5-diyl) (P3HT). Different from the arrangement in a complete OSC sketched in Fig. 2, the P3HT is used pure and not applied in form of a bulk hetero-junction material mixed with an electron acceptor like Phenyl-C61-butyric acid methyl ester (PCBM). anion incorporation -.1V +.75V hν hν -.1 V extinction V +.6 V +.75 V wavelength / nm Fig. 4: The reduced (upper left) and the oxidized (upper right) form of the p-conducting polymer P3HT. Between -.1 and.75 V the oxidation state of the P3HT film can be changed by ex- or incorporation of anions. In both the reduced as well as the oxidized state the film may absorb photons (middle). The absorption shifts from the higher energy of the reduced form to lower energy in the near IR for the oxidized states forming bi-polarons. The P3HT exists mainly in two forms which differ in the oxidation state. Fig. 4 upper left shows the reduced form, which can be excited by photons with a relative high energy, forming the absorption band around 525 nm in the spectrum displayed in Fig. 4 middle. In this state the film appears relatively opaque lilac. The oxidized form appears almost transparent in VIS with a green tone, due to the broad absorption band beginning at about 65 nm with a flat maximum in the near IR around 8 nm. In the original work the automatic measurement campaign SER was performed like displayed in the following Table.

5 KIT 212 CIMPS-abs 4 LPS POL EIS AS Linear Potential Scan 1mV/s between last set-point potential and next setpoint potential. Potentiostatic polarization at the setpoint potential for 1 min to establish steady state settling. Electrochemical Impedance Spectroscopy 1MHz 1mHz 1MHz. 5mV amplitude UV-VIS-NIR Absorption Spectroscopy nm Recording of the DC current history Table: Components of the Automatic Series Measurement Campaign SER 1.5 Current / µa 1.5 LPS: Voltage = ± 5 mv Voltage Scan Rate = ± 1 mv/s Evaluated Charge Integral Q LPS current / na 3 1 POL for Steady State Settling. Evaluated Charge Integral Q POL Evaluated Saturation Current time / s Potential / mv Potential / V steps from -.1V to +.75V and back Fig. 5: Two pre-treatment phases are used within the SER. Every step between the set voltages is 5mV wide and is swept within 5 sec. The data of LPS as well as of the setting phase are stored to protocol the charge history

6 KIT 212 CIMPS-abs 5 impedance / Ω 3K 1K 3K 1K EIS Spectrum: Frequency Range scanned twice: 1 MHz 1mHz phase / o absorption / % Absorption Spectrum: Darkscan UV-VIS-NIR Spectrum with Sample Cell UV-VIS-NIR Spectrum with Reference Cell m K 1K 1K 1M frequency / Hz wavelength / nm Potential / V steps from -.1V to +.75V and back Fig. 6: Spectral Resolved Techniques within the SER: EIS records (left) and optical absorption spectra (right). At each voltage set point repetitive actions of pre-treatment (Fig. 5) and measurements (Fig. 6) are executed. From time requirement reasons on the one hand, and from stability reasons at the other hand, the demonstration experiment cannot be performed fully identical to the original work. Instead, the SER campaign is executed just one time (a total of three spectra of each type) at an intermediate potential around +5mV. The recorded data and spectra will be discussed on the basis of the original data.

7 KIT 212 CIMPS-abs 6 The Experimental Set Up The practical set up consists of the following components: Standard CIMPS system White light LED Broadband spectrometer PECC2 photo electrochemical cell with Acetonitrile / TBA-PF 6 electrolyte and Ag/AgCl 3m-NaCl reference electrode TCO-PEDOT:PSS-P3HT multilayer sample as working electrode in a PECC2 2 nd PECC2 as optical reference cell, containing only electrolyte + TCO glass Automatic slide supporting the change between measuring and reference cell The standard CIMPS components LDA, light source potentiostat and feedback photodiode are connected in the usual way described for standard CIMPS with the EPC Channel 1 routed to the light source potentiostat, which drives the LDA with the white LED illuminator (Fig. 7). Electrochemical workstation Light source supply potentiostat UV/VIS/NIRspectrometer White LED light source Feedback sensor for automatic intensity control Photo-electrochemical reference and measurement cell Actuator for automatic change between reference- and measurement cell Fig. 7: Set-up and connection scheme of CIMPS-abs The photo-sensor head of an ILT9 wideband UV-VIS-NIR spectrometer is placed in the optical axis behind the PECC2, recording the light passing through the sample cell respectively through the reference cell. The spectrometer is connected to the PC which drives also the Zennium Electrochemical Workstation via the USB.

8 KIT 212 CIMPS-abs 7 The Experimental Procedure The hardware is set up like described above. Besides using the standard CIMPS-abs software, a special script source file is loaded into the script panel and compiled. The source code is displayed in the following: '***********************************' ' Manual start for testing purposes ' '***********************************' SCRIPT1 N%=34 forr%=ton% pushr%,n% gosubprior 'call pre-treatment section gosubafter 'call post-treatment section next gotosc_end '**********************************************' 'Pre-treatment and electrochemical measurements' '**********************************************' PRIOR:: bm$="c:\flink\pics\temp\temp.bmp" plot"dm",,,639,511,bm$ pullsc_i%,sc_c% Uset=Ustart b=-(sc_i%>mod%) f=sc_i%*(1-b)+(mod%*2-sc_i%)*b b=-(sc_c%>mod%) d=sc_c%*(1-b)+mod%*b ifsc_c%thenuset=ustart+f*(uend-ustart)/d POTENTIAL lprintpact,uset':gotonext1 mateckpot()=uset EckPot()=Pact pusheckpot(),uset packn$,using"@@",sc_i% NN$="p3ht_pedot" MEAS_EXE("pullEckPot(),PO_P1(,)") POTENTIAL Pset=Pact:Pot=-1 SETUPECW 'sweep to the next set-point MEAS_IE MEAS_SAVE_IE(65,"@"+GP$+NN$,NN$+N$) 'record the current settling at the set-point MEAS_POL MEAS_SAVE_POL(65,"@"+GP$+NN$,NN$+N$) Ampl=5:Pot=-1:Pset=Uset SETUPECW 'record the impedance spectrum at the set-point MEAS_EIS MEAS_SAVE_EIS(65,"@"+GP$+NN$,NN$+N$) NEXT1:: gosubfrees plot"bm",,,bm$ return

9 KIT 212 CIMPS-abs 8 '*********************************************' 'Post-treatment: simply check break conditions' '*********************************************' AFTER:: ifsc_c%=sc_i%trueif Pot= SETUPECW endif return START:: ifinit%=trueif incinit% dimeckpot(3) Ustart=-.1:Uend=.75:Mod%=18-1 GP$="c:\temp\" GETPARAM GP$="c:\eis21\messungen\" MEAS_OPEN_POL(65,GP$,"test_pol") MEAS_OPEN_IE(65,GP$,"test_ie") MEAS_OPEN_EIS(65,GP$,"test_eis") endif INBOX() INBOX$("Scan values") INBOX$("Starting potential",fnstr$(ustart),1,-4,4) INBOX$("Ending potential",fnstr$(uend),1,-4,4) INBOX$("Modulo",fnSTR$(Mod%+1),17,1,999) INBOX(1,3,25,5) iffl%=1thenreturn Ustart=fnVAL(i$(1)) Uend=fnVAL(i$(2)) Mod%=fnVAL(i$(3))-1 return SC_END:: SCRIPT_END Essential are the sections with the label PRIOR and AFTER. They will be automatically targeted when the CIMPS-abs is started using the count modus of series recording. Details upon the scripting techniques are subject of the other courses. Fig. 8: Setting the pre-treatment / post-treatment script to range values, reasonable for the training experiment The pre-treatment / post-treatment script should be adjusted to the scan values, displayed in Fig. 8. The total scan will then run over about 8 minutes. The script button #1 is reserved for testing purposes and should not be used. The CIMPS-abs control panel is used to adjust the conditions and to trigger the measurement campaign.

10 KIT 212 CIMPS-abs 9 Fig. 9: Entering the Series Parameter Configuration Menu (left), selection of the parameter count (middle) and input of the number of counts (right). As a series condition parameter the type vs. count is used (Fig. 9). In this mode, the CIMPS-abs software automatically calls the procedures PRIOR and AFTER as sub-routines before and after each absorption spectrum, if a corresponding script is present and compiled. In order not to overstress the reversibility of the sample and to save time in the training experiment, a count of three is recommended. Fig. 1: Adjusting the data file storage path / name for the optical spectra Before finally starting the SER measurement campaign by means of the Absorbance Series button (Fig. 11), the path and name for the resulting absorption spectra has to be defined (Fig. 1). The spectra present from previous runs should be deleted before. Fig. 11: Starting the SER campaign

11 KIT 212 CIMPS-abs 1 The options for the execution of automatic dark scan and automatic reference scan should be set by means of the corresponding check boxes (Fig. 11). During the training session, the acquired absorption spectra will be displayed and discussed using the light-spectra analysis package of THALES. Due to the complexity of the multi layer system, the analysis of the impedance spectra is not trivial. Therefore already defined and tested equivalent circuit models will be used for demonstration and discussion. -.1V -.5V impedance'' / KΩ V impedance' / KΩ V +.7V +.65V impedance'' / Ω impedance' / Ω Fig. 12: Upper part: modelling & fit of the reduced state spectra (left) and the model used (right). Components: 1,2: inert hole transport layer with 3, porous distribution. 4,5: active layer redox Faraday impedance, 6 film assigned diffusion, 7 layer capacity with 8, porous distribution. 9: electrolyte resistance. Lower part: modelling & fit of the oxidized states (left) and the model used (right). Components: 1,2: (slightly oxidized) hole transport layer with 3, porous distribution. 4,5: (almost) fully oxidized active layer. 6: electrolyte resistance. Fig. 12 shows the modeling for the fully reduced and fully oxidized state of the polymer film. A section through the whole voltage scan is shown in Fig. 13.

12 KIT 212 CIMPS-abs 11 1K +.3V -.1V V -.1V 1K impedance / Ω 1K 1 phase / o V V 1m K 3K 1K 1K frequency / Hz 1m K 3K 1K 1K frequency / Hz Fig. 13: Equivalent circuit fit along the whole oxidation state cycle using the models of Fig. 12. The samples belong to the measurement data, the solid lines to the model calculation.

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